HRID2072302

反应详情

EQUATION

反应方程式

HRID 2072302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

28 ml of boron trifluoride etherate is added to a suspension of 46 g of crude 3-benzylmercapto-4-carbomethoxy benzoic acid in 750 ml of anhydrous tetrahydrofuran and 7 g of sodium borohydride. The reaction mixture is stirred for 3-4 hours at room temperature, then diluted with about 20 ml of 2N hydrochloric acid and 500 ml of water. The product obtained is extracted with ether and the ether extract is washed with water and saturated sodium chloride solution, dried over sodium sulfate and evaporated to dryness. Crystallization from ethyl acetate:hexane (1:2) yielded 28.6 g of 3-benzylmercapto-4-carbomethoxy benzyl alcohol having a melting point of 89.5°-92° C.

WORKUP

后处理

  1. customThe product obtained
  2. extractionis extracted with ether
  3. extractionthe ether extract
  4. washis washed with water and saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated to dryness
  7. customCrystallization from ethyl acetate:hexane (1:2)