反应详情

6.78 g (20 mmol) of 4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one was heated to 100° in a pressure tube overnight with 80 mg of bis-(triphenylphosphine)-palladium(II) dichloride, 30 mg of copper(I) iodide and about 2 ml of propyne in 60 ml of diethylamine. The reaction mixture was then evaporated and the residue was chromatographed on 300 g of silica gel while eluting with ethyl acetate. By recrystallization of the crude product from ethanol there was obtained 4,5-dihydro-5-methyl-3-(1-propynyl)-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 206°-207°.

1. customThe reaction mixture was then evaporated
2. customthe residue was chromatographed on 300 g of silica gel
3. washwhile eluting with ethyl acetate
4. customBy recrystallization of the crude product from ethanol