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[ CAS No. 598-55-0 ] {[proInfo.proName]}

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Chemical Structure| 598-55-0
Chemical Structure| 598-55-0
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Quality Control of [ 598-55-0 ]

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Product Details of [ 598-55-0 ]

CAS No. :598-55-0 MDL No. :MFCD00007964
Formula : C2H5NO2 Boiling Point : -
Linear Structure Formula :- InChI Key :GTCAXTIRRLKXRU-UHFFFAOYSA-N
M.W : 75.07 Pubchem ID :11722
Synonyms :

Calculated chemistry of [ 598-55-0 ]      Expand+

Physicochemical Properties

Num. heavy atoms : 5
Num. arom. heavy atoms : 0
Fraction Csp3 : 0.5
Num. rotatable bonds : 1
Num. H-bond acceptors : 2.0
Num. H-bond donors : 1.0
Molar Refractivity : 16.11
TPSA : 52.32 ?2

Pharmacokinetics

GI absorption : High
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) : -7.23 cm/s

Lipophilicity

Log Po/w (iLOGP) : 0.91
Log Po/w (XLOGP3) : -0.66
Log Po/w (WLOGP) : -0.29
Log Po/w (MLOGP) : -0.96
Log Po/w (SILICOS-IT) : -0.9
Consensus Log Po/w : -0.38

Druglikeness

Lipinski : 0.0
Ghose : None
Veber : 0.0
Egan : 0.0
Muegge : 2.0
Bioavailability Score : 0.55

Water Solubility

Log S (ESOL) : 0.18
Solubility : 113.0 mg/ml ; 1.5 mol/l
Class : Highly soluble
Log S (Ali) : 0.03
Solubility : 81.4 mg/ml ; 1.08 mol/l
Class : Highly soluble
Log S (SILICOS-IT) : 0.53
Solubility : 257.0 mg/ml ; 3.42 mol/l
Class : Soluble

Medicinal Chemistry

PAINS : 0.0 alert
Brenk : 0.0 alert
Leadlikeness : 1.0
Synthetic accessibility : 1.18

Safety of [ 598-55-0 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P201-P202-P264-P280-P305+P351+P338-P312-P337+P313-P405-P501 UN#:N/A
Hazard Statements:H302+H312-H319-H351 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 598-55-0 ]

* 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 [ 598-55-0 ]

[ 598-55-0 ] Synthesis Path-Downstream   1~11

  • 1
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  • [ 57-13-6 ]
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YieldReaction ConditionsOperation in experiment
dibutyldimethoxytin; In Triethylene glycol dimethyl ether; at 111.657 - 161.101℃; for 22h;Compresed liquid(s);Conversion of starting material; EXAMPLE 3 This Example illustrates the actual production of DMC by one step. The reboiler of the distillation still was charged with 125 g methyl carbamate, 120 g methanol, 80 g triglyme and 25 dibutyltin dimethoxide. The reboiler temperature was maintained at 349-357 F. by controlling the overhead pressure during the 12 hours uninterrupted run. The flow rate of the overhead liquid product was set at 2 cc/min. A urea solution prepared by dissolving 105.6 g urea in 2200 g methanol was pumped into the reboiler to maintain a constant liquid level in the reboiler. The reaction was terminated after 12 hours uninterrupted operation. The result of this experiment is listed in Table 2. The change of the DMC composition in the overhead products is shown in FIG. 3. The overhead pressures at the beginning and the end of 12 hours run were 66 and 134.7 psig, respectively. The column temperatures at the bottom and top section of the column were 248 F. and 233 F. at the beginning, and 286 F. and 274 F. at the end of 12 hours, respectively. While the analysis of the sample taken from the reboiler a the end of 12 hours run indicated 3.8% dimethyl carbonate, 20.9% methanol, 21.1% methyl carbamate, 1.5% N-MMC, 52.0% triglyme, 0.2% unknown, 0.2% methylamine (or water) and 0.3% ammonia, the overhead product contained 9.0% dimethyl carbonate, 88.4% methanol, 0.1% methylamine (or water) and 2.5% ammonia. The content of urea in the bottom product sample was unknown because urea could not be analyzed by gc due to urea decomposition. The unit was shut down for the next day's run. The weight of the composite overhead product was 1054 g and the weight of the urea solution pumped into the reboiler was 1252 g. The total samples taken out from the unit was 210.8 g. There was lower liquid level in the reboiler from 8 to 12 hours on stream. The composite overhead product contained 11.5% dimethyl carbonate. A vent gas was collected for 12 hours during the reaction (very little gas volume) and the analysis of this vent gas indicated 0.05 vol % CO2 and 2.1 vol O2 indicating very little decomposition of methyl carbamate or urea. Samples of the overhead product were taken hourly over the duration of the run. The DMC concentration in these samples is illustrated in FIG. 3. The result of this experiment is summarized in Table 2. The maximum concentration of DMC was -16 wt % in the 5 hr sample. The productivity observed at 5 hr was assumed to be indicative of the space yield that could be achieved with the system under steady state conditions. The value was calculated to be -3.4 lb DMC/hr-ft3 (2 g/min×0.16/350 cm2×60 min/hr×2.2E-0.3 lb/g×2.832E+04 cm3/ft3). This value was used in sizing the reaction zone of the reactive distillation column. The run was continued the next day by pumping a mixed solution prepared by mixing 1650 g methanol with 142.5 g triglyme into the reboiler. The reboiler temperature was maintained at 348-359 F. by controlling the overhead pressure. The flow rate of the overhead liquid product was set a 2 cc/min. The reaction was terminated after 10 hours uninterrupted operation. The result of this experiment is listed in Table 2. The overhead pressures at the beginning and the end of 10 hours uninterrupted run were 232.1 and 201.7 psig, respectively. The column temperatures at the bottom and top section of the column were 248 F. and 233 F. at the beginning, and 322 F. and 313 F. at the end of 10 hours run, respectively. While the analysis of the sample taken from the reboiler at the end of 10 hours (total 22 hours from the very beginning) run indicated 1.7% dimethyl carbonate, 22.2% methanol, 1.5% methyl carbamate, 1.3% N-MMC, 71.9% triglyme, 1.3% unknowns and 0.1% air, the overhead product contained 3.8% dimethyl carbonate, 94.94% methanol and 1.2% ammonia. The content of urea in the bottom product sample was unknown, because urea could not be analyzed by gc due to urea decomposition. The weight of the composite overhead product was 956 g and the weight of the mixed solution pumped into the reboiler was 1088. The total weight of the samples taken out from the unit was 197.2 g. The total weight of the inventory material collected from the column and the reboiler was 249. The vent gas was collected during the run (very small gas volume) and it contained 10.0 vol% CO2 and 0.7 vol O2.
  • 2
  • [ 67-56-1 ]
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  • [ 616-38-6 ]
  • [ 74-89-5 ]
YieldReaction ConditionsOperation in experiment
dibutyldimethoxytin; at 160.546 - 178.323℃; for 12h;Compresed liquid(s);Conversion of starting material; The reaction was carried out in the reboiler (350 ml) of a distillation still. The distillation column was ? diameter and 18 long, which was packed with ceramic saddles. The reboiler was charged with 125 g MC (methyl carbamate), 200 g methanol and 25.3 g dibutyltin dimethoxide. The reboiler temperature was maintained at 355-363 F. by controlling the overhead pressure. The flow rate of the overhead product was set at 1.5 cc/min. Methanol was continuously pumped into the reboiler to maintain a constant liquid level in the reboiler. The reaction was carried out for 6 hours each day for 2 days, for a total of 12 hours. After a 6 hour run, the unit was shut down. On the following day the unit was restarted. During the reaction the overhead liquid products were collected into a reservoir. At the end of the run all the composite overhead liquid product in the reservoir and the inventory materials in the reboiler and column were removed from the system and weighted and then analyzed. During the run the samples taken from the unit for analysis were also weighted. The result is listed in Table 1. The change in the compositions of DMC and methylamine in the overhead liquid products during the run is illustrated in FIGS. 1 and 2, respectively. The overhead pressure at 355 F. at the beginning and the end were 268.4 and 374.4 psig, respectively. The column temperatures at the bottom and top section of the column were 332 F. and 321 F. at the beginning, and 353 F. and 348 F. at the end of 12 hours run. The analysis of the bottom product sample taken from the reboiler at the end of 12 hours indicated trace ammonia, 6.9% DMC, 3.6% N-MMC, 2.1% MC, 86.6% methanol, and 0.7% others. The overhead product contained 2.1% DMC and 2.5% methylamine. The content of urea in the bottom product sample was unknown because urea could not be analyzed by gas chromatography due to urea decomposition.
dibutyldimethoxytin; In Triethylene glycol dimethyl ether; at 93.3233 - 142.212℃; for 12h;Compresed liquid(s);Conversion of starting material; The reboiler of the distillation still was charged with 125 g MC, 100 g methanol, 100 g triglyme and 24.7 g dibutyltin dimethoxide. The reboiler temperature was maintained at 355-363 F. by controlling the overhead pressure. The flowrate of the overhead liquid product was set at 1.5 cc/min. To maintain a constant liquid level in the reboiler, a mixture of methanol and triglyme was prepared by mixing 1650 g methanol with 142.5 g triglyme was continuously pumped into the reboiler. The reaction was carried out for 6 hours each day for 2 days, for a total of 12 hours. The result of this experiment is listed in Table 1. The change in the compositions of DMC and methylamine in the overhead liquid products during the run are illustrated in FIGS. 1 and 2, respectively. The overhead pressures at 355 F. at the beginning and the end were 53.4 psig and 139 psig, respectively. The column temperatures at the bottom and top section of the column were 234 F. and 200 F. at the beginning, and 288 F. and 277 F. at the end of 12 hours run. The analysis of the bottom product sample taken from the reboiler at the end of 12 hours run indicated 0.1% ammonia, 4.1% DMC, 0.3%N-MMC, 2.7% MC, 32.6% methanol, and 60.2% triglyme. The overhead product contained 6.9% dimethyl carbonate. The content of urea could not be analyzed by gas chromatography due to decomposition of urea. Example 2 demonstrates the superior yield and selectivity for DMC of the present invention compared with the prior art (the Example 1). It also demonstrates that the reaction can be carried out under much lower pressure in the presence of the high boiling electron donating oxygen containing solvent, resulting in fast removal of the products DMC and ammonia from the reaction zone as soon as they are produced. Because of the fast removal of the products DMC and ammonia from the reaction zone and the novel organotin complex catalyst Bu2Sn(OCH3)2.chiL (chi=1 or 2), the superior selectivity to DMC is obtained. The DMC content in the overhead liquid product of the present invention was at least 3 times higher than the dibutyltin dimethoxide catalyst alone and in the absence of the solvent triglyme (Example 1). Consequently the separation of dimethyl carbonate from the overhead product can be achieved at much lower cost and much reduced amount of material recycle. The low reactor pressure and non-corrosive reaction system results in a great cost advantage from prior systems.
  • 3
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  • [ 827-16-7 ]
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YieldReaction ConditionsOperation in experiment
dibutyldimethoxytin; In Triethylene glycol dimethyl ether; at 173.879℃; under 5311.07 Torr; for 1500h; The purpose of this experiment is demonstrating a primary reactor system, which is composed of multiple reactors. The same experimental set-up in Example 2 was used to demonstrate the performance of the second primary reactor. The experiment was carried out in the similar manner to the Experiment 2. The present example differs from the Example 2 in that the 8 wt. % DMC solution in methanol is used herein in the place of pure methanol in the Experiment 2 and a slightly lower overhead pressure (88 psig) in the present distillation column. The reboiler of the distillation column was loaded with the following materials; 285 grams of triglyme, 40 grams of methanol and 100 grams of dibutyltin dimethoxide. A steady state operation of the distillation column reactor was obtained, while pumping in MC solution and DMC-methanol solution to the reactor. The reactor operation was continued for more than 1500 hours without interruption at 345 F. for the liquid reaction medium in the reboiler, the distillation column temperature of 278 F., and 88 psig for the overhead column pressure. The average compositions of the overhead and bottom products from the reactor during the 54 hours from 1428 hours to 1482 hours of on-stream-time are listed in Table 2. During this period, the pumping rate of a 22.5 wt. % MC solution (590 ppm H2O) was fixed at 1.97 ml/min and the pumping rate of a 8 wt. % DMC solution (80 ppm H2O) was about 3.2 ml/min at 345 F. The mole ratio of MC/CH3OH and DMC wt. % based on MC and CH3OH in the liquid medium in the reactor are 0.915 and 6.40 wt. % respectively. The result of the experiment corresponds to better than 93 mole % of MC to DMC.
  • 4
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YieldReaction ConditionsOperation in experiment
dibutyldimethoxytin; In Triethylene glycol dimethyl ether; at 173.879℃; under 5455.88 Torr; for 926h; A one liter stirred autoclave serves as the reaction zone and reboiler for the reaction/distillation column reactor, which is connected to a 1 inch diameter×3.5 feet long distillation column. The distillation column has three zone heaters, which are independently controlled. The overhead vapor stream from the distillation column is diluted with a nitrogen stream (800 cc/min) and then partially cooled to about 200 F. with hot water in a condenser. The vapor stream from the condenser cooled to ambient temperature to prevent the plugging problem of a cold spot and overhead backpressure regulator. The liquid stream from the condenser flows to a small overhead liquid reflux drum. The temperature of the liquid reflux drum is maintained at ambient temperature. The flow of the liquid product from the overhead reflux drum is monitored with a LFM (liquid flow meter). The liquid stream from the overhead reflux drum and the cooled vapor stream are combined as product stream from the reaction/distillation reactor. Samples are taken for analyses to determine the composition of the overhead vapor stream coming out of the column. Also occasionally samples are taken from the reboiler to monitor the composition of the liquid reaction medium. Whenever the samples are taken from the reboiler, the make-up solutions are pumped in to compensate for the loss of triglyme and catalyst. During the operation of the reactor, the liquid level inside the reboiler is maintained at a constant level. A vertical sight glass is attached to the reboiler for the visual observation of the liquid level inside the reboiler during the operation. Also the reboiler is equipped with a liquid level digital monitor for the automatic control of the reactor during the night and weekends for unattended operation. To carry out the operation of the primary reactor to produce DMC, a MC feed solution (methyl carbamate in methanol) and a methanol feed are pumped in and combined into a single stream. The combined feed stream is passed through a prereactor (a vertically mounted tubular reactor up-flow) at 300 F. and 230 psig to remove water in the feed streams and then introduced to the primary reactor. The temperature of the liquid reaction medium is controlled by adjusting the overhead pressure of the distillation column and the concentration of high boiling solvent in the reboiler of the distillation column. The products DMC, ammonia and other light by-products such as dimethyl ether and CO2 are boiled off from the liquid medium and carried away along with methanol vapor. The operation of the distillation column is carried out in the unconventional mode to perform partial condensation of the vapor coming out of the liquid medium in the reboiler without liquid reflux from the overhead reflux drum by controlling the vapor temperature, which is done by controlling the zone temperatures of the column with three column zone heaters, while the vapor is coming up the distillation column. It was discovered that the unconventional column operation keeps the triglyme solvent in the reactor and continuously removes the by-product N-MMC along with MC from the liquid reaction medium as a part of the overhead stream, which allows the operation of the reactor for an extended period of time. It is found that no liquid reflux from the overhead reflux drum is highly preferred in minimizing the formation of the by-product N-MMC and heterocyclic compounds. It was possible to operate the reaction/distillation column reactor more than 1000 hours without interruption until a high pressure nitrogen valve to the reboiler was accidentally opened. Operating the distillation column in the conventional way causes shutdown or removal of materials from the reboiler, because of the overflow of the reboiler due to the accumulation of the reaction by-products such as N-MMC, cyanuric acid and TTT (1,3,5-trimethyl triazine-2,4,6-trione), etc. Other critical factors to minimize the side-reactions while maintaining an acceptable DMC production rate are balancing the concentrations of solvent and catalyst, the temperature of liquid medium and the overhead column pressure. The range of optimum operation for the reboiler temperature and the overhead column pressure is from about 330 to about 355 F. for the reboiler temperature and from about 80 to about 110 psig respectively. Detailed Description of the Experiment The reboiler of the distillation column was loaded with the following materials; 285 grams of triglyme, 100 grams of methanol and 100 grams of dibutyltin dimethoxide. A steady state operation of the reaction/distillation column reactor was obtained, while pumping in the 13.3 wt. % MC solution in methanol (280 ppm H2O) at a fixed rate of 3.01 ml/min and about 1.92 ml/min of methanol (80 ppm H2O) at 345 F. for the liquid reaction medium in the reboiler, 260 F. for the vapor temperature in the top section of the distillation column, and 90.8 psig for the overhead column pressure. The flow rate...
YieldReaction ConditionsOperation in experiment
(step [A]) A 500-milliliter three-necked flask fitted with a stirrer, a reflux condenser and a thermometer was charged with 236.3 g (2.00 mols) of methyl 2-hydroxyisobutyrate, 60.1 g (1.00 mol) of urea and 1.5 g of lead oxide, and the mixture was heat-refluxed at 140C and 700 torr while being stirred. After the reaction was conducted for 3 hours, the temperature of the reaction solution reached 170 C Thereaction solution was cooled to obtain 247.7 g of the reaction solution. The composition of the reaction solution was analyzed through liquid chromatography. Consequently, unreacted methyl 2-hydroxyisobutyrate was 104.3 g, 5,5-dimethyl-2,4-oxazolidinedione formed was 121.9 g, byproduct 2-hydroxyisobutyric acid amide was 11.8 g, and by-product methyl carbamate was 3.1 g.
  • 6
  • [ 598-55-0 ]
  • [ 131184-73-1 ]
  • [ 1194551-53-5 ]
  • 7
  • [ 67-56-1 ]
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  • [ 6642-30-4 ]
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YieldReaction ConditionsOperation in experiment
With KNO3/K2O supported on activated cenosphere; at 180℃; for 8h; Methyl carbamate (MC) 7.5 g (100 mmol), methanol 64 g (2000 mmol) and 1 g of KNO3/K2O supported on activated cenosphere. KNO3 supported on activated cenosphere (450C) followed by calcination at 500C for 2h and 600C for 6h) were charged to a 300 ml reactor. The contents were heated to 180C with slow stirring. After attaining the temperature stirring speed was increased to 1000 rpm and the time was noted as zero time. The reaction was continued for 8 hours. Ammonia formed during the reaction was removed using cooled high pressure condenser (condenser was cooled to 15C) fitted above the gas outlet valve of the reactor. Ammonia was removed at the interval of 1 hour during the course of the reaction. After 8 h reaction the reactor was cooled to 25C. Reaction mixture was analyzed by Gas Chromatography and 21.1% MC conversion, 29% selectivity to DMC, and 9.3% selectivity to MMC was observed in the reaction.
With Ce-Co calcined hydrotalcite (CeCoHTlc, Ce2+/Co3+ = 2); at 190℃; for 8h; Methyl carbamate (MC) 7.5 g (100 mmol) and methanol 64 g (2000 mmol) were charged to a 300 ml reactor with lg of calcined CeCoHTlc (x=2). The contents were heated to 190C with slow stirring. After attaining the temperature stirring speed was increased to 1000 rpm and the time was noted as zero time. The reaction was continued for 8 hours. Ammonia formed during the reaction was removed using cooled high pressure condenser (condenser was cooled to 15C) fitted above the gas outlet valve of the reactor. Ammonia was removed at the interval of 1 hour during the course of the reaction. After 8 h reaction the reactor was cooled to 25C. Reaction mixture was analyzed by Gas Chromatography. 70.5% of conversion of MC was observed with 7.5% selectivity towards dimethyl carbonate (DMC) and 22.2% selectivity towards methyl N-methyl carbamate.
With 1-butyl-3-methylimidazolium chloride; at 190℃; for 8h; Example 2: Synthesis of DMC in the presence of (C4MImCI): [0035] Methyl carbamate (MC) 7.5 g (100 mmol) and methanol 64 g (2000 mmol) were charged to a 300 ml reactor with l g of IL (C4MImCl). The contents were heated to 190 C with slow stirring. After attaining the temperature stirring speed was increased to 1000 rpm and the time was noted as zero time. The reaction was continued for 8 hours. Ammonia formed during the reaction was removed using cooled high pressure condenser (condenser was cooled to 15 C) fitted above the gas outlet valve of the reactor. Ammonia was removed at the interval of 1 hour during the course of the reaction. After 8 h reaction the reactor was cooled to room temperature. Reaction mixture was analyzed by Gas Chromatography. 15.1 % of conversion of MC was observed with 19.5% selectivity towards dimethyl carbonate (DMC) and 22.7% selectivity towards MMC (Table 2).
With 1-butyl-3-methylimidazolium Tetrafluoroborate; at 190℃; for 8h; Example 2: Synthesis of DMC in the presence of (C4MImCI): [0035] Methyl carbamate (MC) 7.5 g (100 mmol) and methanol 64 g (2000 mmol) were charged to a 300 ml reactor with l g of IL (C4MImCl). The contents were heated to 190 C with slow stirring. After attaining the temperature stirring speed was increased to 1000 rpm and the time was noted as zero time. The reaction was continued for 8 hours. Ammonia formed during the reaction was removed using cooled high pressure condenser (condenser was cooled to 15 C) fitted above the gas outlet valve of the reactor. Ammonia was removed at the interval of 1 hour during the course of the reaction. After 8 h reaction the reactor was cooled to room temperature. Reaction mixture was analyzed by Gas Chromatography. 15.1 % of conversion of MC was observed with 19.5% selectivity towards dimethyl carbonate (DMC) and 22.7% selectivity towards MMC (Table 2).
With samarium(III) trifluoromethanesulfonate; at 180℃; under 12411.9 - 12929 Torr; for 8h;Inert atmosphere; Methyl carbamate (MC) 228 g (3040 mmol) and methanol 147.5 g (4609 mmol) with 3g of Sm(CF3S03)3were charged to a 2000 ml Parr reactor connected to a nitrogen reservoir from gas inlet valve. The reservoir is fitted to reactor through constant pressure regulator which is set at 250 psi. A back pressure regulator was fitted to reactor at gas outlet valve. Back pressure regulator is set at 240 psi. The pressure difference of 10 psi was maintained between constant pressure regulator and back pressure regulator to ensure positive flow of nitrogen. This will help in stripping of CH3OH along with NH3 that is formed during reaction. The reactor was then pressurized with nitrogen atmosphere at 250 psi. The inlet valve was closed at this point keeping outlet valve open. The contents were heated to 180 C under stirring condition. After attaining the temperature the inlet valve was opened and methanol feeding was started at 7 ml/min. The reaction was continued 8h. During this period methanol along with NH3 was expelled due to the set positive pressure of nitrogen. This methanol along with dissolved NH3 was collected in a trap (cooled with ice and salt mixture) connected to BPR outlet. After completion of reaction the reactor was cooled to 25C. Reaction mixture from reactor as well as from trap was analyzed by Gas Chromatography. From GC analysis 58.12% conversion of methyl carbamate and 73.67% selectivity to DMC and 7.85% selectivity to MMC was observed in the reaction.

  • 8
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  • [ 598-55-0 ]
  • methyl cis-2-(3,4-difluorophenyl)cyclopropylcarbamate [ No CAS ]
  • methyl trans-2-(3,4-difluorophenyl)cyclopropylcarbamate [ No CAS ]
  • 9
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YieldReaction ConditionsOperation in experiment
With Ca-Al calcined hydrotalcite(CaAlHTlc, Ca2+/Al3+ = 3); at 180℃; for 8h; Urea 7.5 g (125 mmol) and methanol 65 g (2030 mmol) were charged to a 300 ml reactor with lg of calcined CaAlHTlc (x=3). The contents were heated to 180C with slow stirring. After attaining the temperature stirring speed was increased to 1000 rpm and the time was noted as zero time. The reaction was continued for 8 hours. Ammonia formed during the reaction was removed using cooled high pressure condenser (condenser was cooled to 15C) fitted above the gas outlet valve of the reactor. Ammonia was removed at the interval of 1 hour during the course of the reaction. After 8 h reaction the reactor was cooled to 25C. Reaction mixture was analyzed by Gas Chromatography. 88% of conversion of urea was observed with 78 % selectivity towards MC and 1.7% selectivity towards dimethyl carbonate (DMC) and 6.3% selectivity for methyl N-methyl carbamate (MMC).
  • 10
  • [ 67-56-1 ]
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  • [ 598-55-0 ]
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  • 11
  • [ 702-79-4 ]
  • [ 598-55-0 ]
  • 1-methoxycarbonylamino-3,5-dimethyladamantane [ No CAS ]
YieldReaction ConditionsOperation in experiment
49% In a container having an internal volume of 300 mL equipped with a thermometer and a reflux condenser, 7.07 g (43.0 mmol) of <strong>[702-79-4]1,3-dimethyladamantane</strong>, And 24.7 g (154 mmol) of bromine were added, 60 to 70 C with stirring For 12 hours and a half. Of the 25.84 g of the obtained reaction solution, 8.81 g The reaction solution was separated. 8.81 g Of the reaction solution is heated at 20 to 30 C. , And then 7.16 g of methyl carbamate (95.4 mmol) were added, The reaction was carried out at 70 to 80 C. with stirring. After 3.5 hours, the obtained reaction solution was cooled to 5 to 10 C., then 9.6 g of dichloromethane and 24.5 g of 20% sodium sulfite aqueous solution were added and the organic layer was taken out. The obtained organic layer was sequentially washed with an aqueous solution of sodium carbonate and water, and then concentrated under reduced pressure. The obtained concentrate was purified by silica gel column chromatography (ethyl acetate: n-hexane = 5: 1 (volume ratio)) to obtain, as a white solid, 1.72 g of 1-methoxycarbonylamino-3,5-dimethyladamantane was obtained (yield: 49%).
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Similarity: 0.58

Chemical Structure| 4114-31-2

[ 4114-31-2 ]

Ethyl hydrazinecarboxylate

Similarity: 0.58

; ;