反应详情

温度

25 °C

A solution of hexahydro-1-methyl-3-(3-oxocyclohexen-1-yl)-2H-azepin-2-one (150 g) in dichloromethane (750 ml) was warmed to 25° C. Bromine (97.5 g) was added over 40 minutes at 25°-32° C. (occasional water cooling being applied) and the mixture stirred for 2 hours at about 25° C. Water (200 ml) was added and the dichloromethane layer washed with water (100 ml). The aqueous phases were combined and extracted into dichloromethane (2×100 ml). The dichloromethane extracts were combined and the solvent distilled off and replaced with ethyl acetate to keep temperature of 72° C. (750 ml ethyl acetate added; 90 ml distillate collected). The mixture was cooled to room temperature and filtered. The product was washed with 100 ml ethyl acetate and dried to give the title compound (134.3 g) as a crystalline fawn powder, m.p. 184°-189° C. Identical to product of Example 4.

1. washthe dichloromethane layer washed with water (100 ml)
2. extractionextracted into dichloromethane (2×100 ml)
3. distillationthe solvent distilled off
4. additiontemperature of 72° C. (750 ml ethyl acetate added; 90 ml distillate collected)
5. temperatureThe mixture was cooled to room temperature
6. filtrationfiltered
7. washThe product was washed with 100 ml ethyl acetate
8. customdried