反应详情

To a cooled and stirred solution of N-tert-butyl-5-{3-[4-trifluoromethyl-6-(6-trifluoromethyl-pyridin-3-yl)-pyrimidin-2-yl]-phenyl}-thiophene-2-sulfonic acid amide (0.45 g) in dichloromethane (6 ml) was added TFA (6 ml) and the reaction mixture was allowed to stir at room temperature for 15 h. The mixture was evaporated to dryness, poured into 2N Na2CO3 solution (25 ml) and extracted with ethyl acetate (3×50 ml). The combined organic layers were washed with brine (50 ml), dried (MgSO4) and evaporated. Further purification by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (ethyl acetate/heptane) yielded the title compound as a light yellow solid (0.2 g, 38%). MS (ISP) 531.0 [(M+H)+]; mp 250.5° C.

1. temperatureTo a cooled
2. customThe mixture was evaporated to dryness
3. additionpoured into 2N Na2CO3 solution (25 ml)
4. extractionextracted with ethyl acetate (3×50 ml)
5. washThe combined organic layers were washed with brine (50 ml)
6. dry with materialdried (MgSO4)
7. customevaporated
8. customFurther purification by flash chromatography
9. customon silica gel (ethyl acetate/heptane) and crystallization (ethyl acetate/heptane)