Potassium Cyanide → HCID 54376820, 화합물
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]=1참가 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
- distillationis distilled off
- washThe solution is washed with water
- dry with materialdried over magnesium sulphate
- customevaporated
- customBy crystallization from ethyl acetate
출처 및 근거
- ORD 기록
- ord-8e938dbe53b8473391568d2b6a5733e5
- 출처 데이터셋
- uspto-grants-1984_12
- 특허 번호
- US04489003
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