反应详情

To a solution of [3,5-difluoro-4-(4-methoxy-benzylamino)-phenyl]-(4-ethyl-piperazin-1-yl)-methanone (11.8 g, 30.4 mmol) obtained in Step C in methanol (150 ml), palladium black was added, followed by stirring for 24 hours under a hydrogen gas atmosphere. Acetic acid (15 ml) was added, followed by further stirring for 17 hours at room temperature. This was filtered through Celite, and the solvent was distilled off under reduced pressure. This was purified by silica gel column chromatography (dichloromethane/methanol=100/1 to 10/1), to obtain the desired compound as a brown solid (7.42 g, 91%).

1. stirringby further stirring for 17 hours at room temperature
2. filtrationThis was filtered through Celite
3. distillationthe solvent was distilled off under reduced pressure
4. customThis was purified by silica gel column chromatography (dichloromethane/methanol=100/1 to 10/1)