Potassium Cyanide → HCID 54376820, 화합물

HRID 1154461노트

반응식

HRID 1154461 반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[C-]#N.[K+].[O:28]1[CH2:33]CC(O)[CH2:30][CH2:29]1>>[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18][CH:19]3[CH2:30][CH2:29][O:28][CH2:33][CH2:20]3)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

4

실험 절차

A mixture of 3.45 g (10 mmol) of ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 100 mg of powdered potassium cyanide and 10 g (100 mmol) of tetrahydro-2H-pyran-4-ol is heated at 140° for 20 hours, whereupon the excess tetrahydro-2H-pyran-4-ol is distilled off and the residue is taken up in chloroform. The solution is washed with water, dried over magnesium sulphate and evaporated. By crystallization from ethyl acetate there is obtained tetrahydro-2H pyran-4-yl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 226°-227°.

후처리

  1. distillationis distilled off
  2. washThe solution is washed with water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customBy crystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-8e938dbe53b8473391568d2b6a5733e5
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04489003

반응 노트

불러오는 중…