反应详情

A suspension of 132 g. of 4'-chloro-2-hydroxy-4-methoxy-benzophenone in 500 ml. of methanol is cooled to -20° C. in a 2 l. shaking autoclave and treated with 120 ml. of liquid ammonia. The mixture is then shaken at 120° C. for 20 hours under a nitrogen atmosphere. After cooling, the yellow crude product is filtered off under suction and washed with a small amount of methanol. There is obtained 4'-chloro-2-hydroxy-4-methoxy-benzophenone imine, having a melting point of 210°-212° C., which can be used in the next step without further purification. An analytical sample is obtained by recrystallization from methanol and has a melting point of 212°-214° C.

1. additionA suspension of 132 g
2. additiontreated with 120 ml
3. stirringThe mixture is then shaken at 120° C. for 20 hours under a nitrogen atmosphere
4. temperatureAfter cooling
5. filtrationthe yellow crude product is filtered off under suction
6. washwashed with a small amount of methanol