反应详情

A mixture of 311 mg (1 mmol) of ethyl (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 66 mg of potassium cyanide and 10 ml of absolute methanol is heated to boiling under reflux for 6 hours. The mixture is concentrated, a small amount of water is added, the mixture is extracted three times with 10 ml of chloroform each time, dried over magnesium sulphate, evaporated and recrystallised from ethyl acetate/hexane. There is obtained methyl (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 165°-167° C.

1. temperatureis heated
2. temperatureunder reflux for 6 hours
3. concentrationThe mixture is concentrated
4. additiona small amount of water is added
5. extractionthe mixture is extracted three times with 10 ml of chloroform each time
6. dry with materialdried over magnesium sulphate
7. customevaporated
8. customrecrystallised from ethyl acetate/hexane