反应详情

691 mL of acetic anhydride are added to a solution cooled to 10° C. of 1200 g (6.976 mol, 1 eq) of 3-bromoaniline in 6 L of dichloromethane in the presence of 1.07 L (7.67 mol, 1.1 eq) of triethylamine and 25.6 g (0.209 mol, 0.03 eq) of 4-(dimethylamino)pyridine. The reaction medium is stirred at room temperature for 4 hours and then hydrolyzed with 850 mL of 1N hydrochloric acid solution, and the phases are separated by settling. The organic phase is washed with 0.5N hydrochloric acid solution and then with water, and the solvent is evaporated off. After recrystallization from diisopropyl ether/heptane, 1506.1 g of N-(3-bromophenyl)acetamide are obtained in solid form. Yield=100%

1. customhydrolyzed with 850 mL of 1N hydrochloric acid solution, and the phases are separated
2. washThe organic phase is washed with 0.5N hydrochloric acid solution
3. customwith water, and the solvent is evaporated off
4. customAfter recrystallization from diisopropyl ether/heptane, 1506.1 g of N-(3-bromophenyl)acetamide
5. customare obtained in solid form