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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → Benzyl 2-{[(3aS,4S,6R,6aR)-6-methoxy-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl]carbonyl}hydrazinecarboxylate

HRID 1168290
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HRID 1168290 반응식
C(Cl)(=O)C(Cl)=O.[CH3:7][O:8][C@H:9]1[C@@H:13]2[O:14][C:15]([CH3:18])([CH3:17])[O:16][C@@H:12]2[C@@H:11]([C:19]([OH:21])=O)[O:10]1.[C:22]([O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)(=[O:25])[NH:23][NH2:24].C(N(CC)CC)C>ClCCl.O.C(OCC)(=O)C>[CH3:7][O:8][C@H:9]1[C@@H:13]2[O:14][C:15]([CH3:17])([CH3:18])[O:16][C@@H:12]2[C@@H:11]([C:19]([NH:24][NH:23][C:22]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[O:25])=[O:21])[O:10]1
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참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 79242Benzyl carbazateHCID 10932896ST092333

생성물 1

HCID 59094496Benzyl 2-{[(3aS,4S,6R,6aR)-6-methoxy-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl]carbonyl}hydrazinecarboxylate수율 96.3%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

Oxalyl chloride (3.5 ml, 40 mmol) was added to a solution of (3aS,4S,6R,6aR)-6-methoxy-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxole-4-carboxylic acid (Justus Liebigs Ann. Chem., 1974, 11, 1856) (3 g, 13.8 mmol) in dichloromethane (25 ml). The solution was stirred at room temperature for 3 hours and the solvent was then evaporated under reduced pressure. The acid chloride was re-dissolved in dichloromethane (25 ml) and treated with benzyl carbazate (2.3 g, 13.8 mmol) and triethylamine (5.7 ml, 41.4 mmol). After having been stirring at room temperature for 12 hours, the mixture was partioned between ethyl acetate (100 ml) and water (50 ml). The ethyl acetate layer was separated, washed with 1M aqueous citric acid solution (50 ml), saturated sodium hydrogencarbonate solution (50 ml) and brine (50 ml) and dried (anhydrous sodium sulphate). Evaporation of solvent under reduced pressure yielded the title compound as a yellow foam (4.87 g).

후처리

  1. customthe solvent was then evaporated under reduced pressure
  2. dissolutionThe acid chloride was re-dissolved in dichloromethane (25 ml)
  3. stirringAfter having been stirring at room temperature for 12 hours
  4. customThe ethyl acetate layer was separated
  5. washwashed with 1M aqueous citric acid solution (50 ml), saturated sodium hydrogencarbonate solution (50 ml) and brine (50 ml)
  6. dry with materialdried (anhydrous sodium sulphate)
  7. customEvaporation of solvent under reduced pressure

출처 및 근거

ORD 기록
ord-1777e081825e44b9b606ed6aaa1b3f34
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06624158B2

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