反应详情

温度

105 °C

3-(2-Chloro-4-methoxy-phenyl)-2-(2-chloro-pyridin-4-yl)-1,1,1-trifluoro-butan-2-ol (Example 132, 48 mg) was dissolved in 48% aqueous HBr (0.9 m) and stirred at 105° C. (bath temperature) for 4 h. The reaction mixture was then poured on ice-water-brine and sat aq NaHCO3 and extracted with ethyl acetate. The combined organic phases were washed with brine, dried over MgSO4 and evaporated in vacuo. The resulting brown residue was purified by flash chromatography (8 g silica gel, ethyl acetate/heptane 1:4) to give the title compound as off-white semisolid (34 mg). MS (m/e)=364.0 (M−H).

1. additionThe reaction mixture was then poured on ice-water-brine
2. extractionextracted with ethyl acetate
3. washThe combined organic phases were washed with brine
4. dry with materialdried over MgSO4
5. customevaporated in vacuo
6. customThe resulting brown residue was purified by flash chromatography (8 g silica gel, ethyl acetate/heptane 1:4)