反应详情

To a solution of 3-methyl-5-(4-Trifluoromethyl-phenyl)-thiophene-2-carbaldehyde (0.130 g, 0.481 mmole) in THF (5 mL), is injected 3.0 M MeMgBr in ethyl ether (0.27 mL, 0.810 mmole) dropwise. The reaction is stirred for 2 hours. The reaction is quenched with saturated NH4Cl(aq) (10 mL), then the aqueous solution is extracted with ethyl acetate (3×15 mL). The combined organic solution is washed with brine (3×50 mL), dried over Na2SO4 and concentrated. The crude product is purified on a silica gel column, eluting with 0-20% ethyl acetate in hexane and concentrated to provide the titled compound as yellow solid.

1. customThe reaction is quenched with saturated NH4Cl(aq) (10 mL)
2. extractionthe aqueous solution is extracted with ethyl acetate (3×15 mL)
3. washThe combined organic solution is washed with brine (3×50 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe crude product is purified on a silica gel column
7. washeluting with 0-20% ethyl acetate in hexane
8. concentrationconcentrated