反应详情

19.8 g (0.0639 mol) of 7-chloro-8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid were suspended in 100 ml of N,N-dimethylformamide while gassing with argon and treated portionwise at room temperature with 10.9 g (0.0671 mol) of 1,1'-carbonyldiimidazole. After the CO2 evolution had finished the beige suspension was stirred at 50° for 30 min., cooled and treated dropwise at a temperature below 25° within about 10 min. with 20 ml of 25% ammonia. After stirring for 15 minutes the brownish solution obtained was poured into 600 ml of ice-water. The mixture was stirred at room temperature for 30 min. and filtered, whereupon the crystals were rinsed with a total of 200 ml of water. After drying there were obtained 14.4 g (73%) of 7-chloro-8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide as beige crystals; m.p. 292°-294°.

1. temperaturecooled
2. stirringAfter stirring for 15 minutes the brownish solution
3. customobtained
4. stirringThe mixture was stirred at room temperature for 30 min.
5. filtrationfiltered, whereupon the crystals
6. washwere rinsed with a total of 200 ml of water
7. customAfter drying there