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CAS No. :29390-67-8 MDL No. :MFCD03452964
Formula : C42H71NO34 Boiling Point : No data available
Linear Structure Formula :- InChI Key :-
M.W : 1134.00 Pubchem ID :-
Synonyms :

Safety of [ 29390-67-8 ]

Signal Word:Warning Class:
Precautionary Statements:P261-P305+P351+P338 UN#:
Hazard Statements:H302-H315-H319-H335 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 29390-67-8 ]

* 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 [ 29390-67-8 ]

[ 29390-67-8 ] Synthesis Path-Downstream   1~11

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  • 6-deoxy-6-amino-(2-<4-(dimethylamino)phenylazo>benzoyl)-β-cyclodextrin [ No CAS ]
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  • 6-deoxy-6-[2-(2-hydroxy-5-nitrophenyl)benzoylamino]-β-cyclodextrin [ No CAS ]
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YieldReaction ConditionsOperation in experiment
79% With ammonium hydroxide; In water; at 50℃; for 72h; Synthesis of mono-6-deoxy-6-amino^-cyclodextrin (CDNH2): Ammonia solution (30ml) was added into crude CDOTs (3g) and the solution stirred for 3 days at 50 °C. The final solution was recrystallized in cold acetone to give the crude compound CDNH2 which was further purified by cation exchange column with deionized water and 0.1 M (NH4)2C03 aqueous buffer solution with overall yield 79percent. The product were tracked by TLC (1- propanol: ethyl acetate: water: NuEta320 = 3: 1 :2: 1 (v/v)) visualized with CAM solution.
60% In neat (no solvent); at 85℃; for 0.5h;Microwave irradiation; 6-deoxy-6-amino-beta-cyclodextrin 3a was synthesised from 6-o-mono(p-toluenesulfonyl)-beta-CD (6-tosyl-beta-CD) 1 according to the literature procedure reported by our own research group,2 which exploits rapid synthesis using microwave mediated irradiation under solvent free reaction conditions (85°C, 200 W for 30 mins, 60percent yield).
With ammonium hydroxide; In water; at 60℃; for 4h; Mono-tosylated beta-cyclodextrin (0.1 g, 0.08 mmol) was placed in 1 mL of aqueous NH4OH (28percent) and heated at 60° C. for four hours. The reaction was then placed in a mixture of acetone:water (5.4:0.6) and stirred. A solid was recovered by filtration and washed with cold ethanol to afford mono-NH2-beta-cyclodextrin.
With ammonium hydroxide; at 60℃; for 4h; [00133] Mono-tosylated beta-cyclodextrin (0.1 g, 0.08 mmol) was placed in 1 mL of aqueous NH4OH (28percent) and heated at 60 °C for four hours. The reaction was then placed in a mixture of acetone:water (5.4:0.6) and stirred. A solid was recovered by filtration nd washed with cold ethanol to afford mono-NH2-P-cyclodextrin.

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YieldReaction ConditionsOperation in experiment
91% With triphenylphosphine; In N,N-dimethyl-formamide; at 20℃; for 10h; The detailed preparation for the picolinamide-modified beta-cyclodextrin/Pd(II) complex (Pd(II)PCA-beta-CD) is illustrated in Scheme 1. First, mono-6-tosyl beta-cyclodextrin (1, Tos-beta-CD) was obtained by the method of Khan etc (Khan & Pitchumani, 2016). Then, Tos-beta-CD was reacted with NaN3 to form 6-monodeoxy-6-monoazido-beta-CD (2, N3-beta-CD), which was further reduced by triphenylphosphine to give a key intermediate: 6-monodeoxy-6-amino-beta-CD (3). PCA-beta-CD (4) was prepared by condensation of PCA (2-pyridinecarboxylic acid) with NH2-beta-CD using N,N?-dicyclohexylcarbo-diimide (DCC) and 1-hydroxy-1H-benzotriazole (HOBt) in N,N?-dimethylformamide (DMF). The synthesis of PCA-(CH2)nNH-beta-CD (6) was achieved in two simple steps: nucleophilic substitution (from 1 to 5) and amidation (from 5 to 6). Finally, all the obtained ligands were stirred with Pd(OAc)2 at room temperature for 24 h in toluene, and the target complexes Pd(II)PCA-beta-CDs (C1-C3) were obtained as light yellow powders. The water solubility of the 4, 6 ligands and C1, C2, C3 complexes in different temperatures were studied. The results showed the complexes have high solubility in the aqueous solution (see Table 1S in SI). Reaction conditions: (a) TsCl, NaOH, CH3CN, H2O, rt, 2h, 15% yield; (b) NaN3, DMF, 80C, 12h, 93% yield; (c) PPh3, DMF, rt, 10h, 91% yield; (d) DCC, HOBt, DMF, 4h at 0C, 18h at rt, 72-83% yield; (e) Pd(OAc)2, toluene, rt, 24h, 60-70% yield; (f) diamine, 80C, 12h, 30% yield.
90% With 5%-palladium/activated carbon; hydrazine hydrate; In methanol; water; for 0.333333h;Reflux; 6-monoamino-6-monodeoxy-betaCD (Free Base) (1)11.60 g (0.01 mol) of 6-monoazido-6-monodeoxy-betaCD was dispersed cold, with stirring, in H2O:MeOH-4:1 mixture (100 mL). First a suspension of Pd/C (0.58 g, 5% Pd content in 3 mL H2O), and then hydrazine monohydrate (5 g, 5 mL, 0.1 mol) were added and heated under reflux. After 20 min with stirring under reflux, the mixture was cooled to about 50 C., filtered to remove the catalyst and washed three times with water (15 mL). After evaporation of the solvents, the crude product was precipitated in an aqueous solution (50 mL) of NH4OH 25% (2 mL). The crystals were filtered, washed three times with MeOH (10 mL) and dried at 60 C., under reduced pressure (10 mbar) overnight in the presence of P2O5 and KOH. The product (1) obtained in the form of white crystals (10.2 g, 90%) was free from nitride and hydrazine, it was characterized by IR and it was stored under vacuum in the presence of KOH. [0465] (1): m.p.: 203-205 C. (dec.). Rf: 0.26-0.29. [0466] IR (KBr) nu/cm-1: disappearance of the azide band (2105), 3428 (O-H), 2928 (C-H), 1080, 1029 (C-O-C). [0467] 1H-NMR (DMSO-d6): delta=5.78-5.63 (m, 14H), 4.90-4.85 (m, 7H), 4.50-4.45 (m, 6H), 3.66-3.54 (m, 28H), 3.42-3.24 (overlap with HDO, m, 16H). [0468] 13C-NMR (125 MHz, DMSO-d6): epsilon=101.8, 82.9, 81.6, 81.5, 73.0, 72.3, 72.1, 59.9.
85% Compound 3 obtained in (ii) above, (24.1 g, 21 mmol) and Ph3P (27.55 g, 105 mmol) were dissolved in DMF (150 ml). The reaction mixture was stirred at 25 C. for 2 h. Concentrated ammonia solution (48.2 ml) was added and a white precipitate was formed. The reaction mixture was maintained at room temperature for 10 h. The precipitate was then removed by filtration and the solvent was evaporated under reduced pressure. The residue was added to ethanol (1500 ml). The solid precipitate was filtered, washed with ether (100 ml) and dried under high vacuum yielding 20.1 g (85% yield) of 4. TLC analysis of 4 performed on silica plates (EtOAc:2-propanol:conc. NH4OH: water-7:7:5:4) showed one major spot (Rf=0.20). 1H NMR (DMSO-d6) delta: 3.30-3.65 (m, 42H), 4.44-4.46 (m, 6H), 4.83, 4.89 (two d, 7H), 5.62-5.78 (m, 14H). HPLC (Luna 5u NH2 100 A, size 250-4.6 mm, mobile phase 65% acetonitrile-35% H2O, flow 1.2 ml/min), Rt=9.6 min.
65% With triphenylphosphine; In water; N,N-dimethyl-formamide; at 25℃; for 20h; The mono-6-N3-beta-CD (1.5 g, 1.32 mmol) was dissolved in 20 mL of dry DMF and triphenylphosphine(1.7 g, 6.49 mmol) was added and stirred at 25 C for 2 h.Slowly add 7 mL of water and continue the reaction for 18 h. Filter to removethe insoluble content. Slowly drip the clear solution into 300 mL of acetone. Stir for 30 min and filter to obtain cake. Dry it in vacuo to give 0.97g ofwhite powderwith a yield of 65%.
45% Compound 3 (12.53 g; 0.0108 mol; 1 eq.) is dissolved in 800 ml of DMF, in a 2 litre round-bottomed flask. A solution of triphenylphosphine (11.38 g; 0.043 mol; 4 eq.) dissolved in 40 ml of DMF is added slowly. After 3 hours at ambient temperature with stirring, the reaction medium is cooled to 0 C. and 410 ml of 20% aqueous ammonia are added. The reaction medium is stirred overnight at ambient temperature and is then concentrated in a rotary evaporator. The oily residue is taken up in 600 ml of water, and the white precipitate formed is filtered off and washed with water (2*80 ml). The filtrate is then concentrated under vacuum and the solid residue is taken up in a minimum of water and then brought to pH 4.5 (initial pH of 8.9), the insoluble material is filtered off and the filtrate is passed batchwise over Lewatit SP 1080 resin (Merck). Compound 4 is detached with 6% aqueous ammonia and the filtrate is then concentrated in a rotary evaporator and taken up in a minimum of water. The insoluble material is filtered off and the filtrate is precipitated from acetone. After drying under vacuum overnight, 7.25 g of crude product are recovered and again dissolved in water. The insoluble material is filtered off on filter paper and the filtrate is brought to pH 4.5. Half is then passed over a column of Lewatit SP 1080 resin and the rest batchwise. The various fractions are evaporated to dryness and then taken up in a minimum of water and, finally, lyophilized. Compound 4 is obtained with an overall yield over the 2 steps of 45%. TLC: Rf=0.2 eluent: 6% NH4OH/EtOH/BuOH: 5/5/4 (v/v/v) M.p.: 160 C. (decomposition) 1H NMR D2O delta (ppm): 5.2-5.05 (m, 7H, H1-CD); 4.1-3.75 (m, 28H, H3-CD/H5-CD/H6II-VIICD/H6II-VII-CD); 3.75-3.5 (m, 14H, H2-CD/H4-CD); 3.25 (d, 1H, H6I-CD, 3J6-5=10 Hz); 3.05 (d, 1H, H6I-CD, 3J6-5=10 Hz) ESI-MS+: m/z measured at 1134.5 [M+H]+, calculated at 1134.4 for C42H72NO34
32.0% beta-CD-N3 (4.565 g, 3.935 mmol) was dissolved in 30 mL DMF with Ph3P (1.5 g, 5.7 mmol) and stirred at 20 C. for 3 h. NH4OH (20 mL, 30% v/v) was then added and stirred overnight. The mixture was then precipitated in 400 mL acetone and dried under vacuum to give a crude solid product. Yield=3.2 g (71.7%). The crude product was then dissolved in mL H2O and the undissolved beta-CD-N3 was filtered off. This solution was then loaded onto an IEX column (BioRex 70, 100-200 mesh, NH4+ form, partially pressure packed in an empty SNAP 100 g cartridge) and run on a Biotage SP40 system at 15 mL/min 500 mL (3.7 CV) was eluted to remove any unreacted OTs and N3, followed by 1 CV 0.1 M NH4OH, 1 CV 0.5 NH4OH, and 5 CV 1M NH4OH to remove the beta-CD-NH2. Fractions were checked via 80:20 MeOH:H2O TLC with anisaldehyde staining. The appropriate fractions were combined and concentrated by rotary evaporation to give pure product. Yield=1.429 g (32.0%). 1H NMR (300 MHz, D2O, delta): 5.04-4.88 (s, 7H, C1H of CD), 3.94-3.66 (m, 28H, C2H, C3H, C4H, and C5H of CD), 3.63-3.32 (m, 14H, C6H of CD), 3.13-3.05 (d, 1H, NH2), 2.90-2.79 (b, 1H, NH2)
In a 250-mL three-necked round-bottomed flask, bCD (5.0 g,4.4 mmol) was dissolved in 112.5 mL of water by heating to60 C under vigorous stirring.28 After cooling to room temperature,finely powdered 1-(p-toluenesulfonyl)imidazole (3.9 g, 17.7 mmol)was added to the suspension. After 6 h, a solution of sodium hydroxide (2.3 g, 56.3 mmol) in 6.3 mL of water was added over20 min. After 10 min, unreacted 1-(p-toluenesulfonyl)imidazolewas removed by filtration. To the filtrate was added ammoniumchloride (6.1 g, 112.5 mmol) to quench the reaction. The resultingmixture was concentrated by blowing a stream of air across themixture and the product began to precipitate out of the solution.The suspension was filtered, and the solid was washed with icewater and acetone. The vacuum-dried tosyl bCD was obtained in28.2% yield. The mono-tosylated bCD was treated with an equivalentamount of sodium azide in 16 mL of water at 80 C for 5 h.29After cooling, the solution was precipitated with acetone and thenlyophilized. Lyophilized azido bCD and triphenylphosphine (PPh3)(224 mg, 848 lmol) were dissolved in DMF (8 mL) and stirred for2 h at room temperature. After adding 1.6 mL of water, the solutionwas stirred for 3 h at 90 C, and the resulting product was precipitatedwith acetone. Amino bCD was purified by cation-exchangechromatography (CM-Sephadex C25) using 0.5-M ammoniumbicarbonate as a solvent and desalted with Bio-gel P2. The productwas confirmed using 1H NMR spectra.
With triphenylphosphine; In N,N-dimethyl-formamide; at 20℃; for 4h; Triphenyl phosphine (PPh3; 0.175 g, 0.67 mmol) was added to a solution of mono-N3-beta-cyclodextrin (0.35 g, 0.3 mmol) in DMF (6 mL). The reaction was stirred for 4 hours at 20 C. and then poured into acetone. The resulting solid was recovered by filtration and washed with acetone to afford mono-NH2-beta-cyclodextrin.
With triphenylphosphine; In N,N-dimethyl-formamide; at 20℃; for 4h; [00135] Triphenyl phosphine (PPh3; 0.175 g, 0.67 mmol) was added to a solution of mono-N3-P-cyclodextrin (0.35 g, 0.3 mmol) in DMF (6 mL). The reaction was stirred for 4 hours at 20 C and then poured into acetone. The resulting solid was recovered by filtration and washed with acetone to afford mono-NH2-P-cyclodextrin.

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