反应详情

温度

100 °C

The compound obtained in Step 1 of Example 29 (2 g), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (1.62 g), tetrakis(triphenylphosphine)palladium (0.41 g) and potassium carbonate (2.94 g) were suspended in dioxane (10 ml) and water (1 ml), and the suspension was heated under reflux at 100° C. for 61 hours. After leaving to cool, a saturated aqueous sodium bicarbonate solution was added, and the organic layer was extracted with ethyl acetate and dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [ethyl acetate:methanol=10:1 (v/v)] to give 1.88 g of the title compound as a solid.

1. customAfter leaving
2. temperatureto cool
3. extractionthe organic layer was extracted with ethyl acetate
4. dry with materialdried over sodium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customthe residue was purified by silica gel column chromatography [ethyl acetate:methanol=10:1 (v/v)]