反应详情

10.0 g (26.7 mmol) of 7-chloro-4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one, 140 mg of bis-(triphenylphosphine)-palladium(II) dichloride, 40 mg of copper(I) iodide and 3.4 ml (40.3 mmol) of methyl propargyl ether in 100 ml of diethylamine were heated to boiling under reflux for 3.5 hours. The reaction mixture was evaporated and the residue was chromatographed on silica gel while eluting with ethyl acetate. After recrystallization from ethyl acetate there was obtained 7-chloro-4,5-dihydro-3-(3-methoxy-1-propynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 154°-156°.

1. temperatureunder reflux for 3.5 hours
2. customThe reaction mixture was evaporated
3. customthe residue was chromatographed on silica gel
4. washwhile eluting with ethyl acetate
5. customAfter recrystallization from ethyl acetate