反应详情

温度

80 °C

To a solution of 100 mg of [1-(2,4-Dichloro-phenyl)-4-methyl-5-(4-trifluoromethyl-phenyl)-1H-pyrazol-3-yl]-methanol in 3 ml of DMF were added 54 mg of sodium hydride (60% in mineral oil) at room temperature. After 15 min, 100 mg of tetrabutylammonium iodide and 117 mg of 4-(2-Bromo-propionylamino)-benzoic acid methyl ester were added and the reaction mixture was heated to 80° C. for 8 h. After cooling to room temperature and dilution with 1 M aqueous hydrochloric acid the reaction mixture was filtered through a chem Elut® cartridge by eluting with ethyl acetate. The solvents were removed under reduced pressure and the residue was purified by preparative HPLC (C18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA). The fractions containing the product were evaporated and lyophilized to yield a white solid. Yield: 24 mg.

1. temperatureAfter cooling to room temperature
2. filtrationdilution with 1 M aqueous hydrochloric acid the reaction mixture was filtered through a chem Elut® cartridge
3. washby eluting with ethyl acetate
4. customThe solvents were removed under reduced pressure
5. customthe residue was purified by preparative HPLC (
6. washC18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA)
7. additionThe fractions containing the product
8. customwere evaporated
9. customto yield a white solid