HRID1095924

反应详情

EQUATION

反应方程式

HRID 1095924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoromethyltrimethylsilane (2M in THF, 25.80 mL) was added at 0° C. to a solution of 2-(2-chloro-4-methoxy-phenyl)-1-(2-methyl-pyridin-4-yl)-propan-1-one (5.98 g) in THF (100 mL) followed by the addition of tetrabutylammonium fluoride trihydrate (1.32 g). Stirring was continued for 2 hours at r.t. The reaction mixture was cooled, poured into ice and basified with sat. Na2CO3. The aqueous phase was then extracted with ethyl acetate and the organic layer was washed with brine, dried over Na2SO4 and evaporated. The residue was purified by flash chromatography (silica gel, gradient of heptane in ethyl acetate) to give the title compound as a light yellow foam (5.96 g, 80%). MS (m/e)=360.1 [MH+].

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. extractionThe aqueous phase was then extracted with ethyl acetate
  3. washthe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. customevaporated
  6. customThe residue was purified by flash chromatography (silica gel, gradient of heptane in ethyl acetate)