反应详情

A mixture of methanol (275 ml.) and 2-chloroacetamido-5-chlorobenzophenone (154.2 g., 0.5 mol) was heated to reflux with a steady stream of ammonia bubbling in. At reflux 37% formaldehyde solution (237 ml) was fed in over ca. 40 minutes. The reaction mixture was then heated under reflux for 5 hours. The flow of ammonia was stopped and the slurry of crystals was cooled to room temperature, filtered, washed with methanol (2 × 125 ml), hot water (4 × 500 ml) and dried. There was obtained 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (104.6 g., 77.3%), melting at 211.5° to 214.5° C.

1. temperaturewas heated
2. customwas fed in over ca. 40 minutes
3. temperatureThe reaction mixture was then heated
4. temperatureunder reflux for 5 hours
5. filtrationfiltered
6. washwashed with methanol (2 × 125 ml), hot water (4 × 500 ml)
7. customdried