反应详情

A mixture of 3-bromo-5-chloro-2-fluoro-pyridine, (CAN 884494-87-5; 2.0 g, 9.50 mmol), 4-chlorophenylboronic acid (CAN 1679-18-1; 1.5 g, 9.50 mmol); tetrakis(triphenylphoshine)-palladium (0.55 g, 0.48 mmol) and potassium carbonate (2.6 g, 19 mmol) in water (50 mL) and THF (50 mL) was heated at reflux temperature for 18 h. The reaction mixture was cooled, diluted with ethyl acetate, phases were separated and the water phase was extracted with ethyl acetate. The organic phases were pooled, dried with MgSO4 and the solvent was removed in vacuo. The residue was purified by column chromatography (on silica gel with a gradient of heptane to heptane:ethyl acetate=9:1 to yield the title product (2.2 g, 95%) as white solid; MS (ESI): 241.0 (M)+.

1. temperatureat reflux temperature for 18 h
2. temperatureThe reaction mixture was cooled
3. customwere separated
4. extractionthe water phase was extracted with ethyl acetate
5. dry with materialdried with MgSO4
6. customthe solvent was removed in vacuo
7. customThe residue was purified by column chromatography (on silica gel with a gradient of heptane to heptane