反应详情

温度

65 °C

2-(2-Fluorophenyl)-1,5-dimethyl-1H-pyrazol-3(2H)-one To a solution of 2-(2-fluorophenyl)-5-methyl-1H-pyrazol-3(2H)-one (500 g, 2602 mmol) in THF (2500 ml) heated to 58° C. was added iodomethane (163 ml) dropwise over 15 mins and the mixture was stirred at 65° C. for 30 mins. K2CO3 (198 g) was added over 20 mins and stirred for 16 hrs. Further iodomethane (16.3 ml) was added and stirring continued for 1 hr. The resulting mixture was cooled to 0° C., filtered and washed with THF (50 ml). The filtrate was evaporated to dryness and purified by column chromatography, eluting with EtOAc/Heptane to give the title compound as a red solid.

1. stirringstirred for 16 hrs
2. stirringstirring
3. waitcontinued for 1 hr
4. temperatureThe resulting mixture was cooled to 0° C.
5. filtrationfiltered
6. washwashed with THF (50 ml)
7. customThe filtrate was evaporated to dryness
8. custompurified by column chromatography
9. washeluting with EtOAc/Heptane