反应详情

温度

110 °C

Bis(triphenylphosphine)palladium(II) dichloride (0.17 g, 0.24 mmol) was added to a deoxygenated mixture of 3-bromo-2-(3-(4-(methoxycarbonyl)phenyl)-2-methylenebutanamido)pyridine 1-oxide (2.0 g, 5.0 mmol), cesium carbonate (4.03 g, 12.4 mmol) in anhydrous DMF (40 mL). The resulting mixture was heated at 110° C. under nitrogen for 20 h, then cooled and filtered through Celite®. The filter cake was washed with ethyl acetate. The filtrate was concentrated, and partitioned between ethyl acetate and brine (2×). The combined organic layers were dried over anhydrous sodium sulfate and concentrated to give the title compound which was used without further purification in next step.

1. temperaturecooled
2. filtrationfiltered through Celite®
3. washThe filter cake was washed with ethyl acetate
4. concentrationThe filtrate was concentrated
5. custompartitioned between ethyl acetate and brine (2×)
6. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
7. concentrationconcentrated