Trifluoroacetic anhydride → HCID 22914615, compound

Participants

Reaction Steps

7.7 ml (55.3 mmol) of trifluoroacetic anhydride were added dropwise at 5°-8° to a suspension of 13.8 g (50.3 mmol) of 7-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo-[1,5-a][1,4]benzodiazepine-3-carboxamide (EPA 150 040) in 80 ml of dioxan and 20 ml of pyridine. The beige solution obtained was stirred at 5° for 2.5 hours and subsequently poured into 220 ml of ice-water. The resulting precipitate was filtered off. After drying at 70°/10 Torr there were obtained 11 g (85%) of 7-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile as a white powder of m.p. >250°.

Provenance & Evidence