反应详情

温度

100 °C

To a solution of 5-methyl-3-phenyl-1H-pyrazole (1.5 g, 9.48 mmol) in THF (20 mL) and water (20 mL), were added sodium iodide (1.42 g, 9.48 mmol), iodine (3.61 g, 14.22 mmol), and K2CO3 (1.96 g, 14.22 mmol) at room temperature. The reaction was warmed to 100° C. and stirred for 10 h. After cooling to room temperature, the reaction was poured into water and extracted with ethyl acetate, which was washed with 2.0 M aq. sodium thiosulfite and saturated. NaHCO3 successively. The extract was dried over MgSO4 and concentrated under reduced pressure to give a semi-solid, which was recrystallized from 10% ethyl acetate in hexane to give the title compound (1.9 g). LCMS m/z=285.5 [M+H]+.

1. temperatureAfter cooling to room temperature
2. extractionextracted with ethyl acetate, which
3. washwas washed with 2.0 M aq. sodium thiosulfite
4. dry with materialThe extract was dried over MgSO4
5. concentrationconcentrated under reduced pressure
6. customto give a semi-solid, which
7. customwas recrystallized from 10% ethyl acetate in hexane