反应详情

温度

-10 °C

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. The reaction mixture was then stirred at ambient temperature for 2 hours. Subsequently, the solution was stirred with ice water, then extracted with three portions of 50 ml of tert.-butyl methyl ether. The combined organic layers were washed with water, aqueous sodium hydrogen carbonate and brine, and dried over anhydrous sodium sulfate. After evaporation of the solvent, 2.6 g of the title compound was obtained as light brown solid.

1. extractionextracted with three portions of 50 ml of tert.-butyl methyl ether
2. washThe combined organic layers were washed with water, aqueous sodium hydrogen carbonate and brine
3. dry with materialdried over anhydrous sodium sulfate
4. customAfter evaporation of the solvent