HRID630234

反应详情

EQUATION

反应方程式

HRID 630234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of sodium borohydride (0.24 g, 6.32 mmol) in anhydrous THF (40 mL) at 0° C. was added dropwise a solution of methyl 2-(trifluoromethyl)pyridine-3-carboxylate (650 mg, 3.16 mmol) in THF (50 mL). After stirring for 1 hour, the reaction mixture was slowly quenched with 15% NaOH and then diluted with water. Ethyl acetate was added, the reaction mixture was stirred for 10 minutes, and the precipitated white solid was filtered off. The solid was washed with ethyl acetate (3×100 mL). The organic layer was separated, dried over anhydrous sodium sulfate, and filtered. The filtrate was evaporated to provide [2-(trifluoromethyl)pyridin-3-yl]methanol as a thick oil (0.505 g, 90% yield), which was used for the next step without any further purification; M+177.1.

WORKUP

后处理

  1. customthe reaction mixture was slowly quenched with 15% NaOH
  2. additiondiluted with water
  3. additionEthyl acetate was added
  4. stirringthe reaction mixture was stirred for 10 minutes
  5. filtrationthe precipitated white solid was filtered off
  6. washThe solid was washed with ethyl acetate (3×100 mL)
  7. customThe organic layer was separated
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. customThe filtrate was evaporated