反应详情

温度

60 °C

A 5 N aqueous sodium hydroxide solution (79 mL) was added to a solution of ethyl 5-[2-fluoro-4-(2-methoxy-3,5-dimethylpyridin-4-yl)phenyl]-1-[(S)-tetrahydrofuran-3-yl]-1H-pyrazole-4-carboxylate (43.2 g) in ethanol (574 mL) at mom temperature, and the reaction mixture was stirred at 60° C. for two hours and 10 minutes. The reaction mixture was cooled to room temperature and then concentrated to half volume under reduced pressure. Water (300 mL) was added to the residue, and ethanol was distilled off under reduced pressure. MTBE (130 mL) was added to the resulting residue, and the aqueous layer was separated. The organic layer was extracted with water (30 mL). The combined aqueous layers were made acidic with 5 N hydrochloric acid (78 mL) under ice-cooling and extracted with ethyl acetate twice. The combined organic layers were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give the title compound (39.0 g).

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated to half volume under reduced pressure
3. additionWater (300 mL) was added to the residue, and ethanol
4. distillationwas distilled off under reduced pressure
5. additionMTBE (130 mL) was added to the resulting residue
6. customthe aqueous layer was separated
7. extractionThe organic layer was extracted with water (30 mL)
8. temperaturecooling
9. extractionextracted with ethyl acetate twice
10. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
11. filtrationfiltered
12. concentrationconcentrated under reduced pressure