反应详情

To a solution of 710 mg of 2-[5-(4-Chloro-phenyl)-1-(2,4-dichloro-phenyl)-4-methyl-1H-pyrazol-3-ylmethoxy]-2-methyl-propionic acid in 5 ml of DMF, 360 mg of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDC), 345 mg of pentafluorophenol and 392 mg of NEM were added and the reaction mixture was stirred for 3 h at room temperature. Then, 353 mg of 4-Aminomethyl-benzoic acid and 540 mg of NEM in 5 ml of DMF were added. After 16 h the reaction mixture was diluted with water and 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: 288 mg.

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