反应详情

A mixture of ethyl 4-({(2E)-3-[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]prop-2-enoyl}amino)benzoate (510 mg), a 2N aqueous sodium hydroxide solution (1.29 mL) and ethanol (20 mL) was stirred at 50° C. for 14 hrs. 1N Hydrochloric acid (2.6 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium hydrogen carbonate, and then with saturated brine, dried (MgSO4) and concentrated. The obtained solid was recrystallized from acetone-hexane to give 4-({(2E)-3-[5-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]prop-2-enoyl}amino)benzoic acid (390 mg, yield 82%) as colorless prism crystals. melting point: 291-292° C.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe ethyl acetate layer was washed with saturated aqueous sodium hydrogen carbonate
3. dry with materialwith saturated brine, dried (MgSO4)
4. concentrationconcentrated
5. customThe obtained solid was recrystallized from acetone-hexane