تفاعل #95640

معادلة التفاعل

5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde-3-oxime

→

5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile

المذيبات

acetic acid anhydride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 28 hours
2. 2
   أخرىAfter evaporation of the mixture in vacuo
3. 3
   غسيلwashed twice with 30 ml of saturated sodium hydrogen carbonate solution each time
4. 4
   تجفيفThe organic phase is dried over magnesium sulphate
5. 5
   أخرىevaporated
6. 6
   أخرىAfter column chromatography on silica gel and recrystallisation from ethyl acetate

الإجراء التجريبي

A solution of 4.8 g (18.7 mmol) of 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde-3-oxime in 50 ml of acetic acid anhydride is heated to boiling under reflux for 28 hours. After evaporation of the mixture in vacuo, the residue is taken up in 150 ml of chloroform and washed twice with 30 ml of saturated sodium hydrogen carbonate solution each time and with 30 ml of water. The organic phase is dried over magnesium sulphate and evaporated. After column chromatography on silica gel and recrystallisation from ethyl acetate, there is obtained 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile of melting point 184°-186° C.

المصدر