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[ CAS No. 24584-09-6 ] {[proInfo.proName]}

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Chemical Structure| 24584-09-6
Chemical Structure| 24584-09-6
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Product Details of [ 24584-09-6 ]

CAS No. :24584-09-6 MDL No. :MFCD00866449
Formula : C11H16N4O4 Boiling Point : -
Linear Structure Formula :- InChI Key :BMKDZUISNHGIBY-ZETCQYMHSA-N
M.W : 268.27 Pubchem ID :71384
Synonyms :
ICRF-187;ADR-529;Zinecard. Foreign brand names: Cardioxane Savene.;US brand names: Totect;Cardioxane;Cardioxan;Zinecard;Totect?;NSC-169780
Chemical Name :4,4'-[(1S)-1-Methyl-1,2-ethanediyl]bis-2,6-piperazinedione

Calculated chemistry of [ 24584-09-6 ]      Expand+

Physicochemical Properties

Num. heavy atoms : 19
Num. arom. heavy atoms : 0
Fraction Csp3 : 0.64
Num. rotatable bonds : 3
Num. H-bond acceptors : 6.0
Num. H-bond donors : 2.0
Molar Refractivity : 78.62
TPSA : 98.82 ?2

Pharmacokinetics

GI absorption : Low
BBB permeant : No
P-gp substrate : No
CYP1A2 inhibitor : No
CYP2C19 inhibitor : No
CYP2C9 inhibitor : No
CYP2D6 inhibitor : No
CYP3A4 inhibitor : No
Log Kp (skin permeation) : -8.93 cm/s

Lipophilicity

Log Po/w (iLOGP) : 0.94
Log Po/w (XLOGP3) : -1.4
Log Po/w (WLOGP) : -4.23
Log Po/w (MLOGP) : -1.15
Log Po/w (SILICOS-IT) : -0.68
Consensus Log Po/w : -1.31

Druglikeness

Lipinski : 0.0
Ghose : None
Veber : 0.0
Egan : 0.0
Muegge : 0.0
Bioavailability Score : 0.55

Water Solubility

Log S (ESOL) : -0.42
Solubility : 101.0 mg/ml ; 0.377 mol/l
Class : Very soluble
Log S (Ali) : -0.17
Solubility : 180.0 mg/ml ; 0.67 mol/l
Class : Very soluble
Log S (SILICOS-IT) : -1.27
Solubility : 14.3 mg/ml ; 0.0535 mol/l
Class : Soluble

Medicinal Chemistry

PAINS : 0.0 alert
Brenk : 1.0 alert
Leadlikeness : 0.0
Synthetic accessibility : 2.31

Safety of [ 24584-09-6 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 24584-09-6 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 24584-09-6 ]

[ 24584-09-6 ] Synthesis Path-Downstream   1~10

  • 1
  • [ 24584-09-6 ]
  • ADR-925 [ No CAS ]
  • {Carbamoylmethyl-[(S)-2-(3,5-dioxo-piperazin-1-yl)-propyl]-amino}-acetic acid [ No CAS ]
  • {Carbamoylmethyl-[(S)-2-(3,5-dioxo-piperazin-1-yl)-1-methyl-ethyl]-amino}-acetic acid [ No CAS ]
YieldReaction ConditionsOperation in experiment
The above are prepared by hydrolyzing 5 mg/ml <strong>[24584-09-6]dexrazoxane</strong> with NaOH (40 mul/ml of 1 M NaOH) at 25° C. for 40 min and quenching the reaction with HCl (45 mul/ml of 1 M HCl) to pH 3 as described previously. Under these conditions a mixture of <strong>[24584-09-6]dexrazoxane</strong>, B, C, and ADR-925 is produced. <strong>[24584-09-6]Dexrazoxane</strong> is efficiently removed from the reaction mixture by loading 500 mul of the mixture on a Sep-Pak Plus C18 cartridge (Waters, Mississauga, ON, Canada) and eluting with 2percent (v/v) methanol at a flow rate of 1 ml/min. Although <strong>[24584-09-6]dexrazoxane</strong> is highly retained on the cartridge, B, C, and ADR-925 eluted together and are collected at elution volumes between 1.5 and 2.5 ml. HPLC analysis confirmed that <strong>[24584-09-6]dexrazoxane</strong> is not detectable in this fraction. This 1-ml fraction, pH 6, is loaded on three Sep-Pak Accell Plus QMA (Waters) ion exchange cartridges connected in series and eluted with 2percent (v/v) methanol at a flow rate of 5 ml/min. Fractions containing B are collected at elution volumes between 3 and 4.5 ml, and those containing C between 5 and 9 ml. The B fraction contains less than 0.1 mol percent and 0.01 mol percent of C and ADR-925, respectively. The C fraction contains less than 0.1 mol percent B and 0.05 mol percent of ADR-925, respectively. These fractions are brought to pH 2 with 5 M HCl and evaporated to dryness under a stream of nitrogen, stored at 80° C., and reconstituted in water just before use. Neither of these fractions contain detectable amounts of <strong>[24584-09-6]dexrazoxane</strong> (<0.001 mol percent). Typical yields of B and C are 10 and 6 mug, respectively.
YieldReaction ConditionsOperation in experiment
Dilute the hot phenolic solution with 10 L of ethanol. Externally cool using brine to about 20° C. with stirring over 2-4 hour period and for a further 12 hours cool to about 15° C. using water. Filter the precipitated crude product and wash four times with 2 L of ethanol. Then slurry with 2 L of ethanol and finally wash with another 2 L of ethanol. Check for the absence of phenol by TLC. Dry for 18-24 hours at 40° C. under vacuum. The yield is about 900 g crude (S)(+)-1,2-bis(3,5-dioxopiperazinyl)propane. (54-61percent). The product was purified as follows: In a 20-L glass vessel, charge 9.0 L of pyrogen-free water or 4.5 L of pyrogen-free water and 4.5 L of ethanol and heat to 85°-95° C. Add about 900 g of crude product and stir rapidly until dissolution is complete (maximum time about 5 minutes). Filter the hot solution through layers of dicalite and decolorizing charcoal and collect the filtrate in a 20-L glass vessel. Cool rapidly to 5° to 10° C. using brine and keep at this temperature for about 1 hour. Filter the crystalline product and wash in succession with approximately 0.8 L of pre-cooled (5° to 10° C.) pyrogen-free water then approximately 1.2 L of pre-cooled (5° to 10° C.) diethyl ether. Dry the product for at least 12 hours at 40° C. under vacuum. Withdraw a sample and place in an air-tight amber glass container. The yield is about 800 g (76-85percent purified). While the invention has been illustrated with respect to the preparation of (S)(+)-1,2-bis(3,5-dioxopiperazinyl)propane, it will be apparent that other compounds within the scope of formula (I) and, more particularly, (R)(-)-1,2-bis(3,5-dioxopiperazinyl)propane can be prepared by analogous processes.
  • 3
  • [ 7647-01-0 ]
  • [ 24584-09-6 ]
  • dexrazoxane hydrochloride [ No CAS ]
YieldReaction ConditionsOperation in experiment
In N,N-dimethyl-formamide; acetonitrile;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
  • 4
  • [ 110-16-7 ]
  • [ 24584-09-6 ]
  • dexrazoxane maleate salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
In 1,4-dioxane; methanol;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
  • 5
  • [ 75-75-2 ]
  • [ 24584-09-6 ]
  • dexrazoxane mesylate salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
for 0.0333333h;Product distribution / selectivity; <strong>[24584-09-6]Dexrazoxane</strong> (ICRF- 187) freebase was dissolved at a concentration of 30 mg/mL in 0.15M methanesulfonic acid or 0.1M sulfuric acid to form mesylate or sulfate salts in situ. <strong>[24584-09-6]Dexrazoxane</strong> dissolved in both acids in about 2 minutes. The mesylate and sulfate salts were then diluted with Plasma-Lyte A, Sodium Lactate orRingers lactate infusion fluids to concentrations of 10 mg/mL and 4 mg/mL.Lyophilized Cardioxane was reconstituted directly with Plasma-Lyte A, Na Lactate or Ringers lactate to concentrations of 10 mg/mL and 4 mg/mL. Upon complete dissolution or reconstitution, the pH of each solution was measured and recorded. The solutions were stored at 25°C or 50C. Stability samples were collected at 0, 2, 4, 6, 8, and 24 hours. Each sample was diluted with HPLC mobile phase to a concentration of about 1.0 mg/mL for HPLC analysis.
In 1,4-dioxane; N,N-dimethyl-formamide;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In N,N-dimethyl-formamide; acetonitrile;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane; water;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane; methanol;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.

  • 6
  • [ 7664-93-9 ]
  • [ 24584-09-6 ]
  • dexrazoxane sulfate salt [ No CAS ]
YieldReaction ConditionsOperation in experiment
for 0.0333333h;Product distribution / selectivity; <strong>[24584-09-6]Dexrazoxane</strong> (ICRF- 187) freebase was dissolved at a concentration of 30 mg/mL in 0.15M methanesulfonic acid or 0.1M sulfuric acid to form mesylate or sulfate salts in situ. <strong>[24584-09-6]Dexrazoxane</strong> dissolved in both acids in about 2 minutes. The mesylate and sulfate salts were then diluted with Plasma-Lyte A, Sodium Lactate orRingers lactate infusion fluids to concentrations of 10 mg/mL and 4 mg/mL.Lyophilized Cardioxane was reconstituted directly with Plasma-Lyte A, Na Lactate or Ringers lactate to concentrations of 10 mg/mL and 4 mg/mL. Upon complete dissolution or reconstitution, the pH of each solution was measured and recorded. The solutions were stored at 25°C or 50C. Stability samples were collected at 0, 2, 4, 6, 8, and 24 hours. Each sample was diluted with HPLC mobile phase to a concentration of about 1.0 mg/mL for HPLC analysis.
In N,N-dimethyl-formamide; isopropyl alcohol;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane; N,N-dimethyl-formamide;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In N,N-dimethyl-formamide; acetonitrile;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane; water;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane; methanol;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.
In 1,4-dioxane;Product distribution / selectivity; Cooling MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 2A). These solvents were chosen such that the <strong>[24584-09-6]dexrazoxane</strong> freebase is soluble in the solvents but the salts formed from the reaction of the freebase and acids when the respective acids are added to the crystallization solvents are not soluble. Equimolar amount of the desired acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent to form a solution. The salt precipitated in the solution. The precipitates, which were typically not crystalline or were partially crystalline are collected through filtration on a filter and dried by vacuum. Methanol was then added to the dried powder and heated to 65°C to dissolve the entire salt. The solution then cooled in a controlled manner to 5°C overnight in RS-IO Chemblock Reaction Station (Barnstead International, Dubuque, IA). The crystals are then harvested on a filter and dried at < 40°C. <n="46"/>Anti-Solvent MethodICRF- 187 freebase was dissolved in the desired crystallization solvent or mixture of solvents (Table 1). Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution but the total solution volume is such that the salt formed in-situ remains dissolved in the solution or is soluble in the solution. While the solution was being gently stirred, an anti-solvent (Table 2A) was slowly added until the salt begins to precipitate from the solution. Additional anti-solvent is added until sufficient salt is formed. The crystals was then harvested on a filter and dried at <4O0C.Solvent Evaporation method ICRF- 187 freebase is dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. With gently stirring, minimum amount of water was added until the salt is completely dissolved. Nitrogen was introduced into the solution and the solvents were slowly evaporated until salt precipitation appeared. Additional anti-solvent is added until sufficient salt is formed. The crystals are then harvested on a filter and dried at < 40°C.Direct precipitation methodICRF- 187 freebase was dissolved in dioxane. Equimolar amount of the acid - i.e. sulfuric, maleic, methanesulfonic or hydrochloric acid - was added to the solvent or mixtures of solvents to form a solution. The salt precipitated in the solution. The crystals are then harvested on a filter and dried at < or = 40°C.X-ray powder diffraction analysesThe XRPD analyses were performed using a Shimadzu XRD-6000 X-ray powder diffractometer using Cu Ka radiation. The instrument was equipped with a long fine focus X-ray tube. The tube voltage and amperage were set to 40 kV and 40 <n="47"/>mA, respectively. The divergence and scattering slits were set at 1° and the receiving slit was set at 0.15 mm. Diffracted radiation was detected by a NaI scintillation detector. A Psi-2Psi continuous scan at 37min (0.4 sec/0.02o step) from 2.5 to 40° 2Psi was used. A silicon standard was analyzed to check the instrument alignment. Data were collected and analyzed using XRD-6000 v. 4.1. The peak lists were generated with the Shimadzu software using default peak picking parameters on smoothed, background-subtracted, Ka1 -corrected traces.

  • 7
  • [ 4408-81-5 ]
  • [ 24584-09-6 ]
YieldReaction ConditionsOperation in experiment
With formamide; at 110 - 160℃; for 6.0h; Propane-1,2-diamine tetra-acetic acid (9 g), and formamide (250 mL) are heated at 110° C. together under reduced pressure (ca 100 mm.) for 2 hours. The heat is then raised to 160° C. and stirred for 3 additional hours. The reaction is cooled until precipitate forms and product is filtered and then washed with formamide and ethanol. Further purification is performed by column chromatography (C11H16N4O4, MH+ 269.3, m.p. 191-197° C.).
  • 8
  • [ 1029441-44-8 ]
  • [ 24584-09-6 ]
YieldReaction ConditionsOperation in experiment
With ammonia; In formamide; at 40 - 150℃; under 3750.38 Torr;Industry scale; 5.2. Cyclization to (S)-(+)-4,4'-(1-methyl-1,2-ethandiyl)-bis-(2,6-piperazinedione) (Dexrazoxan) (I); 4.7 kg of gaseous ammonia are added to a solution of 10 kg (S)-(+)-1,2-diaminopropane-N,N,N',N'-tetraacetic acid methyl ester from the aforementioned example in 34 l formamide and the reaction mixture is maintained at 40 to 50° C. under a pressure of max. 5 bar for about 12 h. Thereafter, the reaction mixture is slowly heated to 150° C., obtained methanol is distilled off during heating and the reaction mixture is maintained at 140 to 150° C. for 10 to 12 h. Then the solvent is distilled off, the oily residue is crystallized from methanol to yield 2.9 to 3.7 kg Dexrazoxan, which may be further purified by recrystallization from 1,4-dioxan.
With sodium hydride; formamide; In 1,4-dioxane; at 50℃; for 24.0h;Inert atmosphere; (S)-1,2-diaminopropane-tetraacetic acid methyl ester (2000 mg, 5.5 mmol, 1 eq, 0.3 M) And a solution of formamide (742 mg, 16.5 mmol, 3 eq) in dioxane (5 ml, treated with sodium) At room temperature was slowly added dropwise to a solution of sodium hydride (660 mg, 16.5 mmol, 3 eq) in dioxane (13 ml, Treated with sodium), reacted at 50 °C under nitrogen for 24 hours, and the reaction was completed. filter, Washed with anhydrous ether (20 ml x 2), the filter cake was added to anhydrous ether (55 ml) The pH was adjusted to 7 with formic acid, filtered, the filter cake was added to dioxane (100 ml, untreated) Stirring at 50 °C for 30 min, filtering, the filtrate was concentrated to dryness, adding a small amount of methanol (2 ~ 3ml) Precipitated solid, filtered, dried, crude crude imine, white powder, crude yield of 66percent.
With sodium methylate; formamide; In methanol; at 20℃; for 72.0h; Sodium methoxide (62 g, 1140 mmol, 4 eq) was added to dry methanol (600 mL).Return to room temperature in solution,Addition of formamide (29 mL, 711 mmol, 2.5 eq) was stirred at room temperature for 1 hour.(S)-1,2-Diaminopropane-tetraacetic acid methyl ester (103 g, 285 mmol, 1 eq) was added dropwise slowly.The anhydrous methanol solution was reacted at room temperature for 72 hours. After the reaction is over,Formic acid (43 mL, 1140 mmol, 4 eq) was added dropwise under a water bath and stirred at room temperature for 1 hour.Filtration, adding the filter cake to dioxane (1 L), stirring at 50 ° C for 30 min,Filter, concentrate the filtrate to dryness, and add a small amount of methanol (100 mL).Precipitate solids, filter,Drain,Obtaining the crude compound of formula I (54.2 g),The yield was 71.6percent.
  • 9
  • [ 21416-67-1 ]
  • [ 24584-09-6 ]
  • (R)-razoxane [ No CAS ]
YieldReaction ConditionsOperation in experiment
With uncoated fused-silica capillaries of 50mm I.D. and a total length of 58.5 cm (50 cm effective length) with chiral carbosilane dendrimer functionalized with N-acetyl-L-cysteine (G1Si(SCH2CH(NHCOCH3)(COOH))8) as chiral selector; In N,N-dimethyl-formamide; at 20℃; for 0.15h;pH 9;Resolution of racemate; At the beginning of each working day the capillary was flushed with NaOH 0.1M for 10min, 5min with Milli-Q water and 40min with the buffer in basic conditions and with MeOH for 5min, NaOH 1M for 25min, 5 min with Milli-Q water, 5min with HCl 0.1M and 30min with the buffer in acid conditions. In order to ensure the repeatability between injections, the capillary was flushed with NaOH 0.1M for 5min, 5min with the buffer and 2min with the BGE in basic or acid conditions. Buffer solutions were prepared by dissolving the appropriate amount of formic acid, acetic acid, ammonium bicarbonate or boric acid in Milli-Q water, adjusting the pH to the desired value (pH 2.5, 5.0, 7.0, or 9.0, respectively) with 0.1 or 1M NaOH before completing the volume with water to get the desired buffer concentration. Finally, BGEs were prepared by dissolving the appropriate amount of the chiral selectors in the buffer solution. Stock standard solutions of racemic captopril, econazole and clenbuterol were prepared by dissolving the appropriate amount of these drugs in MeOH and razoxane was prepared by dissolving the appropriate amount in Milli-Q water/25percent DMF (v/v). These solutions were stored at 4°C. All solutions (buffers and standards) were filtered through 0.45mum pore size nylon membrane filters before their injection in the CE system.
  • 10
  • [ 15250-41-6 ]
  • [ 24584-09-6 ]
YieldReaction ConditionsOperation in experiment
50.2% With formamide; for 4.0h;Reflux; Add 10.0g to the reaction flask(S)-N,N,N',N'-1,2-propanediaminetetraacetic acid (4) and 50 ml of formamide,The reaction was refluxed for 4 h.Excess formamide was distilled off under reduced pressure.Add 30m L of ethanol and stir for 1h.After suction filtration, the solid was washed with ethanol, and ethanol was recrystallized to obtain 4.72 g of solid dexrazoxane (1).The purity is 98.3%. Yield 50.2%,
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[ 24584-09-6 ]

Chemical Structure| 1263283-43-7

A347711[ 1263283-43-7 ]

(S)-4,4'-(Propane-1,2-diyl)bis(piperazine-2,6-dione) hydrochloride

Reason: Free-salt

; ;