反应详情

Methyl-4-(6-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazol-3-ylamine (61 mg, 0.27 mmol) is mixed with N-(3-Bromo-4-methyl-phenyl)-3-trifluoromethyl-benzamide (161 mg, 0.45 mmol), palladium acetate (20 mg, 0.089 mmol), Xantophos (78 mg, 0.135 mmol) and cesium carbonate (280 mg, 0.86 mmol). 2 mL anhydrous 1,4-dioxane is added under nitrogen environment and the mixture is subjected to microwave irradiation to 150° C. for 45 minutes. The reaction mixture is then cooled to room temperature, treated with 100 mL THF, passed through a celite column and concentrated. The crude product is purified by ISCO chromatography eluting with ethyl acetate in hexanes from 10% to 100% to afford N-{4-Methyl-3-[1-methyl-4-(6-methylsulfanyl-pyrimidin-4-yl)-1H-pyrazol-3-ylamino]-phenyl}-3-trifluoromethyl-benzamide.

1. customirradiation to 150° C. for 45 minutes
2. concentrationconcentrated
3. customThe crude product is purified by ISCO chromatography
4. washeluting with ethyl acetate in hexanes from 10% to 100%