تفاعل #95675

معادلة التفاعل

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

المذيبات

acetic acid anhydride

ظروف التفاعل

المعالجة

1. 1
   أخرىthe mixture is evaporated
2. 2
   غسيلthe solution is washed once with saturated sodium hydrogen carbonate solution and once with water
3. 3
   تجفيفThe chloroform solution is dried over magnesium sulphate
4. 4
   تركيزconcentrated
5. 5
   أخرىAfter column chromatography and recrystallisation from ethyl acetate

الإجراء التجريبي

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.

المصدر