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

HRID 2356383

反応式

HRID 2356383 の反応式
[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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-73dba824b6a34dd4a3e3a31b28376924
出典データセット
uspto-grants-2010_07
特許番号
US07759362B2

関連ノート

読み込み中…