反应详情

A solution of 3-(2-chloro-4-methoxy-phenyl)-1,1,1-trifluoro-2-(2-methyl-pyridin-4-yl)-butan-2-ol (2.77 g) in aqueous HBr (48%, 50 mL) was refluxed for 4 hours. The reaction mixture was cooled, poured into ice and basified with sat. Na2CO3 to pH 10. 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 colorless foam (2.34 g, 88%). MS (m/e)=346.1 [MH−].

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)