反应详情

To a solution of 2,6-dibromopyridine (1.25 g, 5.28 mmol) in dimethoxyethane (100 mL) and water (50 mL), was added 4-trifluromethylphenylboronic acid (1 g, 5.27 mmol) and sodium carbonate (1.45 g, 13.7 mmol). The resulting mixture was flushed with nitrogen prior to addition of tetrakis(triphenylphosphine) palladium (0) (60 mg, 0.05 mmol). The reaction mixture was heated to reflux under nitrogen for 5 h and then allowed to attain room temperature. The solvents were removed in vacuo and the residue diluted with water (50 mL) and then extracted EtOAc (2×100 mL). The organic solution was dried (MgSO4), filtered and the solvents removed in vacuo. Purification by Biotage™ chromatography (Silica, 90 g) eluting with 4:1 cyclohexane:chloroform afforded the title compound as a white solid (0.35 g).

1. customThe resulting mixture was flushed with nitrogen
2. temperatureThe reaction mixture was heated
3. temperatureto reflux under nitrogen for 5 h
4. customto attain room temperature
5. customThe solvents were removed in vacuo
6. additionthe residue diluted with water (50 mL)
7. dry with materialThe organic solution was dried (MgSO4)
8. filtrationfiltered
9. customthe solvents removed in vacuo
10. customPurification by Biotage™ chromatography (Silica, 90 g)
11. washeluting with 4:1 cyclohexane