Reaktion #95640

Reaktionsgleichung

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

Lösungsmittel

acetic acid anhydride

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle