反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In 2 ml of dichloromethane, 352 mg (2 mmol) of Boc-aminopropanol and 412 g (2 mmol) of ibuprofen (manufactured by Wako Pure Chemical Industries) were dissolved, and 48 mg (0.4 mmol) of DMAP and 423 g (2.2 mmol) of WSCI.HCl/2 ml dichloromethane were added thereto in this order under ice-cooling. After returning to room temperature and stirring overnight, 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 665 mg of the titled compound (yield 91%). The structure was identified by 1H-NMR (CDCl3).
WORKUP
后处理
- temperaturein this order under ice-cooling
- customAfter returning to room temperature
- customfollowed by separation
- washby washing with 5% citric acid twice
- dry with materialAfter dehydration drying with sodium sulfate, ethyl acetate
- customwas evaporated under reduced pressure