反应详情

温度

100 °C

7-(3,5-Difluorophenyl)-2-methylpyrazolo[1,5-a]pyrimidin-5(4H)-one (521 mg) is dissolved in POCl3 (15 mL) and pyridine (0.2 mL) and stirred overnight while heating at 100° C. After cooling to room temperature, the reaction solvent is removed by distillation under reduced pressure. The remainder is extracted with ethyl acetate and water. The extracted organic layer is washed with 1 M NaHCO3 aqueous solution and brine and dehydrated with anhydrous MgSO4. The dehydrated organic layer is distilled under reduced pressure and purified by column chromatography to yield the target compound (327 mg). 1H NMR (CDCl3, 300 MHz) δ 7.63 (m, 2H), 7.02 (m, 1H), 6.82 (m, 1H), 6.52 (m, 1H), 2.52 (s, 3H).

1. temperatureAfter cooling to room temperature
2. customthe reaction solvent is removed by distillation under reduced pressure
3. extractionThe remainder is extracted with ethyl acetate and water
4. washThe extracted organic layer is washed with 1 M NaHCO3 aqueous solution and brine
5. distillationThe dehydrated organic layer is distilled under reduced pressure
6. custompurified by column chromatography