反应详情

To a solution of 500 mg of [5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-methanol in 6 ml of DMF were added 242 mg of sodium hydride (60% in mineral oil) at room temperature. After 15 min, 448 mg of tetrabutylammonium iodide and 946 mg of 2-Bromo-2-methyl-propionic acid ethyl ester were added and the reaction mixture was stirred for 16 h at room temperature. After dilution with saturated aqueous sodium hydrogen carbonate solution the reaction mixture was filtered through a chem Elut® cartridge by eluting with ethyl acetate The solvents were removed under reduced pressure and the crude product was purified by chromatography on silica gel eluting with a gradient of n-heptane/ethyl acetate. The fractions containing the product were combined and the solvent evaporated under reduced pressure. Yield: 200 mg.

1. filtrationAfter dilution with saturated aqueous sodium hydrogen carbonate solution the reaction mixture was filtered through a chem Elut® cartridge
2. washby eluting with ethyl acetate The solvents
3. customwere removed under reduced pressure
4. customthe crude product was purified by chromatography on silica gel eluting with a gradient of n-heptane/ethyl acetate
5. additionThe fractions containing the product
6. customthe solvent evaporated under reduced pressure