HRID1359977

反应详情

EQUATION

反应方程式

HRID 1359977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 2 ml of dichloromethane, 352 mg (2 mmol) of Boc-aminopropanol and 489 g (2 mmol) of flurbiprofen (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, 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 753 mg of the titled compound (yield 94%). The structure was identified by 1H-NMR (CDCl3).

WORKUP

后处理

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