反应详情

温度

90 °C

To a solution of (S)-4-(1-(3-bromophenoxy)ethyl)-N-((2-hydroxy-4,6-dimethylpyridin-3-yl)methyl)benzamide (0.20 g, 0.44 mmol), 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (0.13 g, 0.59 mmol), tetrakis(triphenylphosphine) palladium(0) (0.05 g, 0.04 mmol) in 1,4-dioxane (10 mL) and water (1.0 mL) was added sodium carbonate (0.14 g, 1.0 mmol). The reaction mixture was stirred at 90° C. for 12 hours. After the reaction, the reaction mixture was poured to the water (100 mL) and the product was extracted by dichloromethane (100 mL), concentrated and purified by column chromatography (silica gel:dichloromethane:methanol=12:1 with 1% ammonia aqueous solution) to give pure product (S)-4-(1-(3-(2-aminopyrimidin-5-yl)phenoxy)ethyl)-N-((2-hydroxy-4,6-dimethylpyridin-3-yl)methyl)benzamide (0.12 g, 60%) as a white solid. LR MS (M+H+): calcd for: 469.21. found 469.

1. customAfter the reaction
2. extractionthe product was extracted by dichloromethane (100 mL)
3. concentrationconcentrated
4. custompurified by column chromatography (silica gel:dichloromethane:methanol=12:1 with 1% ammonia aqueous solution)