반응 #95640

반응 방정식

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

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

용매

acetic acid anhydride

반응 조건

후처리

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

실험 절차

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.

출처