HRID1242355
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- additionSubsequently, the solution was poured onto ice water
- extractionextracted with three portions of 50 ml of tert.-butyl methyl ether
- washThe combined organic layers were washed with water, aqueous NaHCO3-solution and brine
- dry with materialdried over sodium sulfate
- customAfter evaporation of the solvents