Reaktion #95575

Reaktionsgleichung

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

→

8-fluoro-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
   Sonstigethe mixture is evaporated
2. 2
   Waschenthe solution is washed once with saturated sodium hydrogen carbonate solution and once with water
3. 3
   TrocknenThe chloroform solution is dried over magnesium sulphate
4. 4
   Einengenconcentrated
5. 5
   SonstigeAfter column chromatography and recrystallisation from ethyl acetate

Vorschrift

1.65 g (6 mmol) of 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde-3-oxime are heated to boiling under reflux for 4.5 hours in 15 ml of acetic acid anhydride and the mixture is evaporated. The residue is taken up in 100 ml of chloroform and the solution is washed once with saturated sodium hydrogen carbonate solution and once with water. The chloroform solution is dried over magnesium sulphate and concentrated. After column chromatography and recrystallisation from ethyl acetate, there is obtained 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile of melting point 236°-237° C.

Quelle