反应详情

7-[4-(2-butoxyethoxy)phenyl]-N-[4-[hydroxy(4-methylpyridin-2-yl)methyl]-3-trifluoromethylphenyl]-1-trifluoroacetyl-2,3-dihydro-1H-1-benzazepine-4-carboxamide (1.2 g) was dissolved in dichloromethane (50 ml), and to the solution was added 3-chloroperbenzoic acid (0.69 g) under ice-cooling and the mixture was stirred overnight at room temperature. An aqueous solution of sodium thiosulfate was added to the mixture, and the mixture was concentrated and extracted with ethyl acetate. The organic layer was washed with sodium bicarbonate solution, water and saturated brine, and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane), to give 7-[4-(2-butoxyethoxy)phenyl]-N-[4-[hydroxy(4-methyl-1-oxidopyridin-2-yl)methyl]-3-trifluoromethylphenyl]-1-trifluoroacetyl-2,3-dihydro-1H-1-benzazepine-4-carboxamide (1 g) as pale brown oil.

1. temperaturecooling
2. concentrationthe mixture was concentrated
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with sodium bicarbonate solution, water and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off
7. customThe residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane)