HRID1168416

反应详情

EQUATION

反应方程式

HRID 1168416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.8 g of 4-chlorobenzyl cyanide, 10 g of ethyl 2-trifluoromethylbenzoate and 2.9 g of sodium ethylate were added to 100 ml of toluene and then reacted for 8 hours under reflux. The reaction mixture was returned to room temperature and extracted by an addition of 200 ml of water. The aqueous phase was adjusted to pH 6 to 7 with 6N hydrochloric acid and then extracted by an addition of 400 ml of methylene chloride. The organic layer was washed with water and a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 6.3 g of the desired product. The NMR spectrum data of this product were the same as in Reference Preparation Example 3.

WORKUP

后处理

  1. customreacted for 8 hours
  2. temperatureunder reflux
  3. customwas returned to room temperature
  4. extractionextracted by an addition of 200 ml of water
  5. extractionextracted by an addition of 400 ml of methylene chloride
  6. washThe organic layer was washed with water
  7. dry with materiala saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure