反应详情

To a solution of ethyl 3-(4-amino-2-fluorophenyl)propanoate (0.496 g, 2.35 mmol) and N,N-diethyl-2-[(3′-formyl-2,6-dimethylbiphenyl-4-yl)oxy]acetamide (0.725 g, 2.14 mmol) in 1,2-dichloroethane (10 mL) was added acetic acid (0.245 mL, 4.28 mmol), and the mixture was stirred at room temperature for 3 hr. Sodium triacetoxyborohydride (0.907 q, 4.28 mmol) was added to the reaction mixture, and the mixture was stirred at room temperature for 15 hr. Water and 10% aqueous citric acid solution were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (20%-70% ethyl acetate/hexane) to give the title compound (0.978 g, yield 86%) as a yellow oil.

1. stirringthe mixture was stirred at room temperature for 15 hr
2. extractionthe mixture was extracted with ethyl acetate
3. washThe extract was washed with saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (20%-70% ethyl acetate/hexane)