反应详情

0.60 g (26 mmol) of sodium was dissolved in 32 ml of methanol. 1.95 g (28.1 mmol) of hydroxylamine hydrochloride and, after 1 hour, 5.77 g (346 mmol) of (S)-7-fluoro-12,12a-dihydro-9-oxo-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carbonitrile were added at room temperature. The suspension was stirred at 70° for 3.5 hours, cooled to 0° during 30 min. and the crystals were filtered off. By drying the crystallizate there were obtained 6.5 g (100%) of (S)-7-fluoro-12,12a-dihydro-9-oxo-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxamidoxime of m.p. 248°-250°.

1. temperaturecooled to 0° during 30 min.
2. filtrationthe crystals were filtered off
3. customBy drying the crystallizate there