反应详情

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 sequentially washed with water (2×), saturated aqueous sodium bicarbonate solution and brine, and then dried (MgSO4). Concentration provided the title compound as a clear oil (5.38 g).

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