反应详情

Under a nitrogen atmosphere, charge a reactor with 42 kg of (5,6-dihydroimidazo[1,2-a][1]benzazepin-4-one), 15.5 kg of hydroxylamine hydrochloride, 21.5 kg of sodium acetate anhydrous, and 171 kg of methanol. Heat the resulting brown suspension to 60 to 70° C. for 20 h (in process HPLC<3% 5,6-dihydroimidazo[1,2-a][1]benzazepin-4-one). Cool the reaction to 23 to 25° C. and stir for 8 h. Isolate the solid by centrifugation, rinsing with 33 kg of cold methanol. Transfer the resulting solid into a reactor and slurry with 210 kg of water at 85 to 90° C. for 2 h. Isolate the solid by centrifugation, rinsing the solid with 85 kg of water. Dry the resulting solid to give 39.65 kg of 5,6-dihydro-4H-benzo[f]imidazo[1,2-a]azepin-4-one oxime. MS=214 (M+1).

1. temperatureCool
2. customthe reaction to 23 to 25° C.
3. customIsolate the solid by centrifugation
4. washrinsing with 33 kg of cold methanol
5. waitslurry with 210 kg of water at 85 to 90° C. for 2 h
6. customIsolate the solid by centrifugation
7. washrinsing the solid with 85 kg of water
8. customDry the resulting solid