反应详情

3,5,-Dibromo-2-pyridinol (1.47 g, 5.81 mmol), 2-bromo-5-methylpyridine (1.00 g, 5.81 mmol), copper (0.008 g, 0.116 mmol) and K2CO3 (0.883 g, 6.39 mmol) were heated at 180° C. for 18 hrs. The brown reaction mixture was cooled, diluted with EtOAc and stirred with saturated NaHCO3 for 1 hr. The aqueous layer was extracted with EtOAc (2×) and the combined organic extracts were washed with brine, dried (Na2SO4) and evaporated in vacuo. The residue was chromatographed (silica gel, EtOAc: CH2Cl2 10:90 to 30:70 gradient elution) to afford the title compound as a white solid.

1. temperatureThe brown reaction mixture was cooled
2. extractionThe aqueous layer was extracted with EtOAc (2×)
3. washthe combined organic extracts were washed with brine
4. dry with materialdried (Na2SO4)
5. customevaporated in vacuo
6. customThe residue was chromatographed
7. wash(silica gel, EtOAc: CH2Cl2 10:90 to 30:70 gradient elution)