反应详情

温度

90 °C

To a round bottle flask, was added methyl 3-formyl-4-(trifluoromethylsulfonyloxy)benzoate (6300 mg, 20 mmol), 2-fluoro-5-methoxyphenylboronic acid (10 g, 61 mmol), potassium phosphate tribasic (6.6 mL, 81 mmol) (granular) and tetrakis(triphenylphosphine)palladium (2.3 g, 2.0 mmol). The flask was flushed with nitrogen and then 40 mL of DME was added. The resulting mixture was then heated at 90° C. for 6 hours. The reaction mixture was diluted with EtOAc and water. The organic phase was washed with water and brine and then dried over anhydrous sodium sulfate. After filtration, the organic solvent was removed in vacuo to give a residue which was purified by CombiFlash® chromatography to give a yellow solid (5.80 g, 100%). MS ESI m/e: 289.2 (M+H)+.

1. customThe flask was flushed with nitrogen
2. addition40 mL of DME was added
3. additionThe reaction mixture was diluted with EtOAc and water
4. washThe organic phase was washed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationAfter filtration
7. customthe organic solvent was removed in vacuo
8. customto give a residue which
9. customwas purified by CombiFlash® chromatography