反应详情

Methyl 4-bromo-3-hydroxybenzoate (2.1 g, 9.0 mmol), 4-fluorophenyl-boronic acid (2.52 g, 18 mmol), tetrakis(triphenylphosphine)palladium (0.52 g, 0.45 mmol), and 2M aqueous sodium carbonate solution (11 ml) in ethanol/toluene (1:5, 30 ml) were heated at reflux overnight. After cooling the solvent was removed in vacuo and the residue dissolved in EtOAc then washed with sat. aq. sodium bicarbonate and dried over MgSO4. The crude product was purified by column chromatography eluting with 1% MeOH/DCM giving the title compound as a solid (1.9 g). MS(ES): MH+ 247, M-H+ 245.

1. temperatureat reflux overnight
2. temperatureAfter cooling the solvent
3. customwas removed in vacuo
4. dissolutionthe residue dissolved in EtOAc
5. washthen washed with sat. aq. sodium bicarbonate
6. dry with materialdried over MgSO4
7. customThe crude product was purified by column chromatography
8. washeluting with 1% MeOH/DCM giving the title compound as a solid (1.9 g)