HRID890449

反应详情

EQUATION

反应方程式

HRID 890449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.6 g (8.40 mmol) of [2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-acetic acid methyl ester in 15 ml of dry tetrahydrofuran were added under an argon atmosphere within 15 minutes to a stirred suspension of 0.38 g (10 mmol) of lithium aluminium hydride in 5 ml of tetrahydrofuran. The reaction was exothermic. Subsequently, the mixture was stirred at room temperature for 1 hour. Then, 1 ml of ethyl acetate was dropped to the reaction mixture, followed by water, drop after drop, under argon, with stirring and cooling until the gas evolution ceased. The reaction mixture was diluted with 50 ml of ethyl acetate, dried with anhydrous sodium sulfate and filtered. The filtrate was evaporated and the residue was chromatographed on silicagel with a mixture of dichloromethane and tert.-butyl methyl ether (4:1 vol./vol.) as eluent. 1.88 g (79.5% of theory) of 2-[2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-ethanol was obtained as white solid.

WORKUP

后处理

  1. stirringunder argon, with stirring
  2. temperaturecooling until the gas evolution
  3. dry with materialdried with anhydrous sodium sulfate
  4. filtrationfiltered
  5. customThe filtrate was evaporated
  6. customthe residue was chromatographed on silicagel with a mixture of dichloromethane and tert.-butyl methyl ether (4:1 vol./vol.) as eluent