反应详情

2-Methyl-4-(6-methylsulfanyl-pyrimidin-4-yl)-2H-pyrazol-3-ylamine (120 mg, 0.54 mmol) is mixed with N-(3-Bromo-4-methyl-phenyl)-3-trifluoromethyl-benzamide (290 mg, 0.81 mmol), palladium acetate (25 mg, 0.1 mmol), Xantophos (100 mg, 0.17 mmol) and cesium carbonate (530 mg, 1.63 mmol). 10 mL of anhydrous 1,4-dioxane is added under a nitrogen environment and the mixture is subjected to microwave irradiation to 150° C. for one hour. 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-[2-methyl-4-(6-methylsulfanyl-pyrimidin-4-yl)-2H-pyrazol-3-ylamino]-phenyl}-3-trifluoromethyl-benzamide: MS m/z 499.1 (M+1).

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