تفاعل #95615

معادلة التفاعل

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

→

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

المذيبات

acetic acid anhydride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 3 hours
2. 2
   أخرىsubsequently evaporated in vacuo
3. 3
   غسيلthe solution is washed once with ca 30 ml of saturated sodium hydrogen carbonate solution and once with ca 30 ml of water
4. 4
   تجفيفdried over magnesium sulphate
5. 5
   أخرىevaporated
6. 6
   أخرىAfter column chromatography and recrystallisation from ethyl acetate

الإجراء التجريبي

A solution of 5.24 g (18.5 mmol) of (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxaldehyde-1-oxime in 50 ml of acetic acid anhydride is heated to boiling under reflux for 3 hours and subsequently evaporated in vacuo. The residue is taken up in chloroform, the solution is washed once with ca 30 ml of saturated sodium hydrogen carbonate solution and once with ca 30 ml of water, dried over magnesium sulphate and evaporated. After column chromatography and recrystallisation from ethyl acetate, there is obtained (S)-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carbonitrile of melting point 223°-225° C.

المصدر