تفاعل #95802

معادلة التفاعل

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

المذيبات

2-propanol

2-propanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe mixture is evaporated in vacuo
2. 2
   درجة الحرارةheated
3. 3
   درجة الحرارةunder reflux for 22 hours
4. 4
   أخرىAfter evaporation in vacuo
5. 5
   workup.ADDITIONthe residue is treated with water
6. 6
   استخلاصextracted three times with 30 ml of chloroform each time
7. 7
   غسيلThe combined chloroform phases are washed three times with 20 ml of water each time
8. 8
   تجفيفdried over magnesium sulphate
9. 9
   أخرىevaporated
10. 10
    أخرىAfter recrystallisation from ethyl acetate/n-hexane

الإجراء التجريبي

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.

المصدر