Ammonia → HCID 22914318, compound

Participants

Reaction Steps

11.5 g (71 mmol) of 1,1'-carbonyldiimidazole were added portionwise to a suspension of 17 g (64.6 mmol) of 5-methyl-4-oxo-5,6-dihydro-4H-imidazo[1,5-a]thieno[3,2-f][1,4]diazepin-7-carboxylic acid (EP 285 837 A1)in 100 ml of N,N-dimethylformamide. The resulting pale brown solution was heated to 50° during 45 minutes. Subsequently, the solution was cooled to room temperature and 20 ml of aqueous ammonia solution were added dropwise thereto. After stirring for a further 30 minutes the reaction mixture was poured into 100 ml of ice-water and the resulting precipitate was filtered off and rinsed with water, ethanol and subsequently with ether. After drying at 70°/10 Torr there were obtained 15 g (89%) of 5-methyl-4-oxo-5,6-dihydro-4H-imidazo[1,5-a]thieno[3,2-f][1,4]diazepine-7-carboxamide as colourless crystals of m.p. >250°.

Provenance & Evidence