反应详情

A mixture of 7-chloro-5,6-dihydro-6-oxo-4H-imidazo [1,5-a][4,1]benzoxazepine-3-carbonitrile (16.86 g, 0.06 mole), potassium carbonate (13.5 g, 0.9 mole) and hydroxylamine hydrochloride (4.6 g, 0.06 mole) in isopropanol (843 ml) containing water (13.5 ml) was stirred at room temperature for 4 days. The reaction mixture was then concentrated to a volume of 256 ml by distillation, cooled to room temperature and water (256 ml) added. The resulting mixture was cooled at 0° C. for 1 hour and the solid collected, washed with water and dried in vacuo at 50° C. to give the product (12 g, 63%), m.p. 252°-254° C.

1. concentrationThe reaction mixture was then concentrated to a volume of 256 ml by distillation
2. temperaturecooled to room temperature
3. additionwater (256 ml) added
4. temperatureThe resulting mixture was cooled at 0° C. for 1 hour
5. customthe solid collected
6. washwashed with water
7. customdried in vacuo at 50° C.