反应详情

In 1,2-dichloroethane (20) were dissolved methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.0 g), n-butylaldehyde (1.3 ml) and acetic acid (0.41 ml), and to the solution was added sodium triacetoxyborohydride (3.8 g). The mixture was stirred at room temperature overnight, poured into water, neutralized with sodium hydrogen carbonate solution and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried with anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified with silica gel column chromatography (ethyl acetate/hexane) to give methyl 7-bromo-1-butyl-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.9 g) as pale yellow oil.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water and saturated brine
3. dry with materialdried with anhydrous magnesium sulfate
4. customThe solvent was evaporated
5. customthe residue was purified with silica gel column chromatography (ethyl acetate/hexane)