HRID1242355

反应详情

EQUATION

反应方程式

HRID 1242355 的结构方程式

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A solution of 2.55 g (8.63 mmol) of the above prepared [2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-acetic acid in 25 ml of methanol was cooled to −10° C.; 1.88 ml (25.9 mmol) of thionyl chloride was added and the reaction mixture was then stirred at ambient temperature for 2 hours. Subsequently, the solution was poured onto ice water, then extracted with three portions of 50 ml of tert.-butyl methyl ether. The combined organic layers were washed with water, aqueous NaHCO3-solution and brine, and dried over sodium sulfate. After evaporation of the solvents, 2.60 g of the title compound was obtained as light brown solid.

WORKUP

后处理

  1. additionSubsequently, the solution was poured onto ice water
  2. extractionextracted with three portions of 50 ml of tert.-butyl methyl ether
  3. washThe combined organic layers were washed with water, aqueous NaHCO3-solution and brine
  4. dry with materialdried over sodium sulfate
  5. customAfter evaporation of the solvents