反应详情

Palladium(0),tetrakis(triphenylphosphine) (4.69 g, 4.05 mmol) was added to a stirred suspension of 2,5-dichloropyridine (12.0 g, 81.08 mmol), 4-hydroxybenzene boronic acid (11.2 g, 81.1 mmol) and potassium carbonate (11.2 g, 81.1 mmol) in dioxane (100 mL) and water (100 mL). The mixture was refluxed for 2 hours, then partitioned between diethyl ether (100 mL) and water (100 mL). The organics were washed with brine (100 mL), dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with 4% methanol in dichloromethane, to afford the title compound as an off-white solid (15.5 g, 81%).

1. temperatureThe mixture was refluxed for 2 hours
2. custompartitioned between diethyl ether (100 mL) and water (100 mL)
3. washThe organics were washed with brine (100 mL)
4. dry with materialdried over magnesium sulphate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel
7. washeluting with 4% methanol in dichloromethane