反应详情

温度

105 °C

The above-obtained 5-hydroxy-1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)-4,5-dihydropyrazole-3-carboxylic acid ethyl ester (0.546 g) was dissolved in ethanol (11 mL). Acetic acid (0.456 mL) was added to the resultant mixture, followed by stirring at 105° C. for 4 hours. The mixture was cooled in air. Subsequently, the reaction mixture was partitioned by use of saturated aqueous solution of sodium hydrogencarbonate, water, and ethyl acetate. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure. The residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give the title compound as a solid substance (0.516 g, 100%).

1. temperatureThe mixture was cooled in air
2. customSubsequently, the reaction mixture was partitioned by use of saturated aqueous solution of sodium hydrogencarbonate, water, and ethyl acetate
3. dry with materialThe organic layer was dried over sodium sulfate anhydrate
4. filtrationfollowed by filtration
5. customThe solvent was evaporated under reduced pressure
6. customThe residue was purified through silica gel column chromatography (hexane-ethyl acetate)