Sodium amide → HCID 53714193, compound

Participants

Reaction Steps

40.70 g of an equimolar mixture of butyltriphenylphosphonium bromide and sodium amide was stirred at room temperature for 15 minutes in 150 ml of tetrahydrofuran. 20.73 g (80 mmol) of 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde was then added thereto, the mixture was stirred at room temperature for a further 1.5 hours, filtered and the filtrate was evaporated. After chromatography of the residue on silica gel while eluting with cyclohexane/ether/isopropanol (3:3:1) and recrystallization from ethyl acetate and n-hexane there was obtained 8-fluoro-4,5-dihydro-5-methyl-3-(1-pentenyl)-6H-imidazo[1,5-a][1,4]-benzodiazepin-6-one of melting point 150°-151°.

Provenance & Evidence