반응 #613870

반응 방정식

2-Bromo-2-methyl-propionic acid ethyl ester

[5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-yl]-methanol

sodium hydride

→

2-[5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-ylmethoxy]-2-methyl-propionic acid ethyl ester

용매

DMF

반응 조건

후처리

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

실험 절차

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.

출처