HRID1974754

反应详情

EQUATION

反应方程式

HRID 1974754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4-fluorothiophenol (3.64 g, 28.4 mmol) in 50 ml of dry THF at -78° C. is added n-butyllithium (17.8 ml of a 1.6M solution in hexane). After 30 minutes, 2-(2,6-difluorophenyl)-4,4-dimethyloxazoline (5.0 g, 23.7 mmol) in 10 ml of dry THF is added dropwise. The reaction mixture is allowed to warm to room temperature and then is heated to 60° C. for 5.5 hours. After cooling, the reaction mixture is poured into water and then extracted with diethyl ether. The extracts are washed with water and then brine, and dried over MgSO4 to afford the crude product. Chromatography over silica gel eluting with 10:1 hexane/ethyl acetate afforded the subtitle compound.

WORKUP

后处理

  1. temperatureis heated to 60° C. for 5.5 hours
  2. temperatureAfter cooling
  3. extractionextracted with diethyl ether
  4. washThe extracts are washed with water
  5. dry with materialbrine, and dried over MgSO4
  6. customto afford the crude product