反应详情

温度

0 °C

To a stirred solution of 2-(4-iodo-imidazol-1-yl)-6-(3-methyl-4-trifluoromethyl-phenyl)-4-trifluoromethyl-pyrimidine (Example E.73) (1.49 g, 3.0 mmol) in THF (21 mL) was added at 0° C. isopropyl-magnesium chloride lithium chloride (1M in THF, 3.6 mL, 3.6 mmol). The reaction mixture was allowed to stir for 15 min at 0° C., tributyltin chloride (1.27 g, 3.9 mmol) was added, the reaction mixture was stirred at room temperature for 16 h, poured into saturated ammonium chloride solution (70 mL) and extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with brine (70 mL), dried (MgSO4) and evaporated. The crude product was further purified by flash chromatography on alox (ethylacetate/heptane) to yield the title compound (0.33 g, 17%) as a light brown oil. MS (ISP) 663.3 [(M+H)+].

1. customwas added at 0° C.
2. stirringthe reaction mixture was stirred at room temperature for 16 h
3. extractionextracted with ethyl acetate (2×100 mL)
4. washThe combined organic layers were washed with brine (70 mL)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe crude product was further purified by flash chromatography on alox (ethylacetate/heptane)