反応 #95640

反応方程式

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

溶媒

acetic acid anhydride

反応条件

後処理

1. 1
   温度under reflux for 28 hours
2. 2
   その他After evaporation of the mixture in vacuo
3. 3
   洗浄washed twice with 30 ml of saturated sodium hydrogen carbonate solution each time
4. 4
   乾燥The organic phase is dried over magnesium sulphate
5. 5
   その他evaporated
6. 6
   その他After column chromatography on silica gel and recrystallisation from ethyl acetate

実験手順

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.

出典