反应详情

3,5-Dichlorobenzoyl chloride (1.7 g) was added to a solution of 3-amino-7,8-dimethoxy-1-phenoxy-2,3,4,5-tetrahydro-3-benzazepine (2.1 g) in 100 ml dichloromethane containing sodium bicarbonate (3 g). After one hour, the mixture was filtered and concentrated. The solid residue was eluted through silica with 10% ethyl acetate in dichloromethane to yield 2.4 g of light tan solid, mp 182°-184°. This solid was recrystallized from acetonitrile to yield 2 g of white crystals, mp 184°-185°.

1. filtrationthe mixture was filtered
2. concentrationconcentrated
3. washThe solid residue was eluted through silica with 10% ethyl acetate in dichloromethane
4. customto yield 2.4 g of light tan solid, mp 182°-184°
5. customThis solid was recrystallized from acetonitrile