反应详情

温度

70 °C

3-Bromo-2-methylprop-1-ene (4.19 g, 31.0 mmol) and cesium carbonate (13.5 g, 41.3 mmol) were added to a solution of 4-(3-methyl-5-nitrophenyl)-1H-pyrazole (4.20 g, 20.7 mmol) in dimethylacetamide (41 mL) and stirred at 70° C. for 18 h. The mixture was allowed to cool to room temperature, passed through CELITE, washed with methanol, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (0-50% EtOAc/Hexane) to afford 4-(3-methyl-5-nitrophenyl)-1-(2-methylallyl)-1H-pyrazole. MS ESI calc'd. for C14H16N3O2 [M+H]+ 258. found 258.

1. temperatureto cool to room temperature
2. washwashed with methanol
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by column chromatography on silica gel (0-50% EtOAc/Hexane)