反应详情

13.50 g of an equimolar mixture of chloromethyltriphenylphosphonium chloride and sodium amide were stirred for 15 minutes with 50 ml of tetrahydrofuran, whereby the temperature rose to 42°. 6.2 g (25.7 mmol) of 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde were then added portionwise thereto, the mixture was stirred at room temperature for a further hour, filtered and the filtrate was evaporated. After chromatography of the residue on silica gel while eluting with cyclohexane/ether/isopropanol (3:3:1) there was obtained 3-[(Z)-2-chlorovinyl]-4,5-dihydro-5-methyl-6H-imidazo-[1,5-a][1,4]benzodiazepin-6-one of melting point 197°-199°.

1. customrose to 42°
2. filtrationfiltered
3. customthe filtrate was evaporated
4. washAfter chromatography of the residue on silica gel while eluting with cyclohexane/ether/isopropanol (3:3:1) there