HRID2232455

反应详情

EQUATION

反应方程式

HRID 2232455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 39.2 g of triethyloxonium tetrafluoroborate in 325 ml of methylene chloride is treated with 32.5 g of o-trifluoromethyl-benzamide. After stirring at room temperature for 48 hours the reaction mixture is poured on to a mixture of 10% sodium carbonate solution and ice and the resulting mixture is extracted three times with methylene chloride. The combined extracts are then washed twice with 10% sodium carbonate solution, dried over anhydrous sodium sulphate and evaporated under reduced pressure. The oily, brown residue is distilled in a high vacuum. There is obtained pure ethyl o-trifluoromethyl-benzimidate, b.p. 67° C./0.15 mmHg.

WORKUP

后处理

  1. extractionthe resulting mixture is extracted three times with methylene chloride
  2. washThe combined extracts are then washed twice with 10% sodium carbonate solution
  3. dry with materialdried over anhydrous sodium sulphate
  4. customevaporated under reduced pressure
  5. distillationThe oily, brown residue is distilled in a high vacuum