反应详情

A mixture of 5-amino-4-[3-(2-aminosulfonylethenyl)benzoyl]-1-(4-fluorophenyl)-pyrazole (2.1 g, 5.43 mmol) and palladium hydroxide (0.6 g) in methanol (150 ml) was shaken in a Parr apparatus under hydrogen atmosphere at 50 psi. After 4 days, the reaction mixture was filtered through Celite® and the filtrate was concentrated. The residue was purified by flash chromatography (elution gradient: 40-100% ethyl acetate/hexane) to give a crude product which was recrystallized from methanol/ethyl acetate/hexane to give 5-amino-4-[3-(2-aminosulfonylethyl)benzoyl]-1-(4-fluorophenyl)pyrazole (0.95 g, mpt. 170-170.4° C.) as a solid.

1. filtrationthe reaction mixture was filtered through Celite®
2. concentrationthe filtrate was concentrated
3. customThe residue was purified by flash chromatography (elution gradient: 40-100% ethyl acetate/hexane)
4. customto give a crude product which
5. customwas recrystallized from methanol/ethyl acetate/hexane