反应详情

61 mg (1 eq, 0.24 mmol) of 1-(4-bromo-2-fluorophenyl)ethanamine from Stage 1 were dissolved in 4 ml of dichloromethane, and 24 mg (1.1 eq, 23 μl, 0.264 mmol) of propanoyl chloride and 70 mg (2.2 eq, 90 μl) of Hünig's base were added. The mixture was stirred at room temperature for 5 h and then concentrated. The crude product was dissolved in ethyl acetate and washed 1× with 1M HCl, 1× with sat. sodium carbonate solution and then with water, and dried over magnesium sulphate. After concentrating under reduced pressure, the resulting crude product was purified by means of chromatography on silica gel (eluent: cyclohexane/ethyl acetate). 50 mg (67%) of N-[1-(4-bromo-2-fluorophenyl)ethyl]propanamide were obtained.

1. concentrationconcentrated
2. dissolutionThe crude product was dissolved in ethyl acetate
3. washwashed 1× with 1M HCl, 1× with sat. sodium carbonate solution
4. dry with materialwith water, and dried over magnesium sulphate
5. concentrationAfter concentrating under reduced pressure
6. customthe resulting crude product was purified by means of chromatography on silica gel (eluent: cyclohexane/ethyl acetate)