HRID2174629

反应详情

EQUATION

反应方程式

HRID 2174629 的结构方程式

PROCEDURE

实验过程

A solution of 2,4,6-trifluorobenzeneacetic acid (5.00 g, 26.3 mmol) in methanol (25 mL) was stirred at ambient temperature, and thionyl chloride (6 mL, ˜3 eq.) was added dropwise, causing the temperature of the reaction mixture to reach 60° C. The reaction mixture was allowed to cool to ambient temperature and was stirred for 3 h. Water (25 mL) was added with ice cooling. The mixture was extracted with ethyl acetate (2×100 mL). The combined organic phases were washed with water (2×), with saturated aqueous sodium bicarbonate solution and with brine, and dried over MgSO4. Concentration provided the title product as a clear oil (5.38 g).

WORKUP

后处理

  1. customto reach 60° C
  2. extractionThe mixture was extracted with ethyl acetate (2×100 mL)
  3. washThe combined organic phases were washed with water (2×), with saturated aqueous sodium bicarbonate solution and with brine
  4. dry with materialdried over MgSO4
  5. concentrationConcentration