反应详情

To a solution of 2 g of [1-(2,4-Dichloro-phenyl)-4-methyl-5-(4-trifluoromethyl-phenyl)-1H-pyrazol-3-yl]-methanol in 15 ml of DMF were added 997 mg of sodium hydride (60% in mineral oil) at room temperature. After 15 min 1.8 g of tetrabutylammonium iodide and 2.9 g 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: 1.3 g.

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
3. customThe solvents were 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