反应详情

Add acetic anhydride (160 mL) to a solution of 1-(3,5-difluorophenyl)-2-nitroethanol (330 g) and 4-dimethylaminopyridine (18 g) in dichloromethane (1000 mL), at room temperature using a water bath to keep the temperature below 35° C. Add acetic acid over 30 min and stir the reaction mixture overnight. Dilute with dichloromethane (600 mL) and wash with 2% aqueous HCl, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate, dry (magnesium sulfate) and concentrate. Wash the crude with hexanes to give the title compound (220 g).

1. customat room temperature
2. customthe temperature below 35° C
3. washwash with 2% aqueous HCl, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate
4. dry with materialdry (magnesium sulfate)
5. concentrationconcentrate
6. washWash the crude with hexanes