反应详情

温度

80 °C

To a flask were added N-[bis(4-methoxyphenyl)methyl]-5-bromo-3-[(4,6-dimethylpyridin-2-yl)amino]pyridine-2-carboxamide (100 mg, 0.183 mmol) (PrepEx 1.11), tert-butyl [1-(acetylamino)-3-aminopropan-2-yl]carbamate (51 mg, 0.22 mmol), tris(dibenzylideneacetone)dipalladium(0) (17 mg, 0.018 mmol), Xantphos (21 mg, 0.037 mmol) and cesium carbonate (131 mg, 0.402 mmol). 1,4-Dioxane (1 mL) was added, and the reaction mixture was purged with nitrogen for 5 minutes. The reaction mixture was then stirred at 80° C. for 16 hours. The reaction mixture was cooled to room temperature, and then diluted with ethyl acetate and saturated aqueous ammonium chloride. The organics were separated, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by chromatography on silica gel to afford tert-butyl {1-(acetylamino)-3-[(6-{[bis(4-methoxyphenyl)methyl]carbamoyl}-5-[(4,6-dimethylpyridin-2-yl)amino]pyridin-3-yl)amino]propan-2-yl}carbamate. MS ESI calc'd for C38H48N7O6 [M+H]+ 698. found 698.

1. customthe reaction mixture was purged with nitrogen for 5 minutes
2. temperatureThe reaction mixture was cooled to room temperature
3. additiondiluted with ethyl acetate and saturated aqueous ammonium chloride
4. customThe organics were separated
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by chromatography on silica gel