Ammonia → HCID 22914329, compound

Participants

Reaction Steps

2.7 g (16.8 mmol) of 1,1'-carbonyldiimidazole were added portionwise to a suspension of 4.7 g (16.0 mmol) of 8-chloro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid in 25 ml of N,N-dimethylformamide. After the CO2 evolution had finished the mixture was heated to 60° for 45 min. Subsequently, the solution was cooled to room temperature and 3.9 ml of conc. aqueous ammonia solution were added dropwise thereto. After stirring for a further 90 minutes the reaction mixture was poured into 90 ml of ice-water and stirred for 1 hr. The white crystals were filtered off under suction and washed with a small amount of water. After drying in a high vacuum there were obtained 3.84 g (83%) of 8-chloro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide of m.p. 275°-277°.

Provenance & Evidence