反应 #95802

反应方程式

potassium cyanide

ethyl (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

potassium cyanide

→

isopropyl (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

溶剂

2-propanol

2-propanol

反应条件

后处理

1. 1
   其他The mixture is evaporated in vacuo
2. 2
   温度heated
3. 3
   温度under reflux for 22 hours
4. 4
   其他After evaporation in vacuo
5. 5
   workup.ADDITIONthe residue is treated with water
6. 6
   萃取extracted three times with 30 ml of chloroform each time
7. 7
   洗涤The combined chloroform phases are washed three times with 20 ml of water each time
8. 8
   干燥dried over magnesium sulphate
9. 9
   其他evaporated
10. 10
    其他After recrystallisation from ethyl acetate/n-hexane

实验过程

934 mg (3 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 are stirred at 60° C. for 48 hours with 198 mg (3 mmol) of potassium cyanide in 30 ml of dry 2-propanol. The mixture is evaporated in vacuo. The residue is treated with 30 ml of 2-propanol and 198 mg (3 mmol) of potassium cyanide and heated to boiling under reflux for 22 hours. After evaporation in vacuo, the residue is treated with water and extracted three times with 30 ml of chloroform each time. The combined chloroform phases are washed three times with 20 ml of water each time, dried over magnesium sulphate and evaporated. After recrystallisation from ethyl acetate/n-hexane, there is obtained isopropyl (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 207°-208° C.

来源