Acetyl chloride → cis-8-Benzyl-2-acetyl-2,8-diazabicyclo[4,3,0]nonane

HRID 2356383

반응식

HRID 2356383 반응식
[CH2:1]([N:8]1[CH2:16][C@@H:15]2[C@@H:10]([CH2:11][CH2:12][CH2:13][NH:14]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17](Cl)(=[O:19])[CH3:18]>ClCCl.C(N(CC)CC)C.C(Cl)(Cl)Cl>[CH2:1]([N:8]1[CH2:16][C@@H:15]2[C@@H:10]([CH2:11][CH2:12][CH2:13][N:14]2[C:17](=[O:19])[CH3:18])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 2

HCID 6367Acetyl chlorideHCID 10198297(4aS-cis-)-6-benzyl-octahydropyrrolo(3.4-b)pyridine

생성물 1

HCID 67237118cis-8-Benzyl-2-acetyl-2,8-diazabicyclo[4,3,0]nonane수율 85.5%

시약·촉매·용매 3

HCID 6212Chloroform용매HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

The preparation comprises dissolving cis-8-benzyl-2,8-diazabicyclo[4,3,0]nonane (5.0 g, 23.1 mmol) in dichloromethane (50 mL) and triethylamine (5 mL) under stirring in ice bath, dropwise adding a solution of acetyl chloride (1.8 g, 23.1 mmol) in chloroform (10 mL), continuing with the stirring until the reaction finishes, distilling off the solvent, and chromatographing on silica gel with petroleum ether and ethyl acetate to give cis-8-benzyl-2-acetyl-2,8-diazabicyclo[4,3,0]nonane (5.1 g, 85.5%).

후처리

  1. distillationdistilling off the solvent, and chromatographing on silica gel with petroleum ether and ethyl acetate

출처 및 근거

ORD 기록
ord-73dba824b6a34dd4a3e3a31b28376924
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07759362B2

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