反应详情

A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and reflux condenser was charged with 1,4-dioxane (60 mL), 111e (crude, 14.1 mmol), 3,5-dibromo-1-methylpyridin-2(1H)-one (4.5 g, 16.9 mmol) and cesium carbonate (11.5 g, 35.2 mmol). After bubbling nitrogen through the resulting solution for 30 min, Xantphos (820 mg, 1.41 mmol) and tris(dibenzylideneacetone)dipalladium(0) (645 mg, 0.7 mmol) were added, and the reaction mixture was heated at reflux for 15 h. After this time the reaction was cooled to room temperature, filtered and concentrated to afford a black solid as the crude product. Then it was purified on silica gel (DCM: MeOH=100:1 to 50:1) to afford 111g as a yellow solid (3.1 g, yield 50%).

1. customA 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer
2. temperaturereflux condenser
3. customAfter bubbling nitrogen through the resulting solution for 30 min
4. temperaturethe reaction mixture was heated
5. temperatureat reflux for 15 h
6. filtrationfiltered
7. concentrationconcentrated
8. customto afford a black solid as the crude product
9. customThen it was purified on silica gel (DCM: MeOH=100:1 to 50:1)