反应详情

To a solution of 4-boronobenzoic acid (1.66 g, 10 mmol) and 2-bromopyridine (1.72 g, 11 mmol) in acetonitrile (40 mL) and water (40 mL), potassium carbonate (5.5 g, 40 mmol), bis(triphenylphosphine)palladium(II) chloride (400 mg, 0.37 mmol) were added. The mixture was degassed and purged withed nitrogen. The mixture was stirred under reflux for 24 h. Then the hot suspension was filtered and concentrated to half of the original volume and washed with dichloromethane. The aquatic phase was adjusted to pH=4 with hydrochloric acid (1 M) and filtrated, washed with water. The residue was dried in vacuum to obtain 1.81 g of white solid of 4-(pyridin-2-yl)benzoic acid. Yield: 91%. LC-MS (ESI) m/z: 200 (M+1)+.

1. customThe mixture was degassed
2. custompurged
3. temperatureunder reflux for 24 h
4. filtrationThen the hot suspension was filtered
5. concentrationconcentrated to half of the original volume
6. washwashed with dichloromethane
7. filtrationfiltrated
8. washwashed with water
9. customThe residue was dried in vacuum