反应详情

In 14 ml of dichloromethane, 2.371 g (13.5 mmol) of Boc-aminopropanol and 3.441 g (13.5 mmol) of ketoprofen (manufactured by Tokyo Kasei Kogyo) were dissolved, and 323 mg (2.6 mmol) of 4-dimethylaminopyridine (DMAP) and 2.833 g (14.8 mmol) of water-soluble carbodiimide hydrochloride (WSCI.HCl)/14 ml dichloromethane were added thereto in this order under ice-cooling. After returning to room temperature and stirring overnight, dichloromethane was evaporated under reduced pressure, and ethyl acetate was added thereto, followed by separation by washing with 5% citric acid twice, water, 5% sodium hydrogen carbonate twice, water and saturated brine consecutively. After dehydration drying with sodium sulfate, ethyl acetate was evaporated under reduced pressure to give 5.430 g of the titled compound (yield 98%). The structure was identified by 1H-NMR (CDCl3).

1. temperaturein this order under ice-cooling
2. customAfter returning to room temperature
3. customdichloromethane was evaporated under reduced pressure, and ethyl acetate
4. additionwas added
5. customfollowed by separation
6. washby washing with 5% citric acid twice
7. dry with materialAfter dehydration drying with sodium sulfate, ethyl acetate
8. customwas evaporated under reduced pressure