反应详情

To a mixture of methyl 3-bromo-5-(methylsulfonyl)benzoate (0.65 g, 2.2 mmol), p-tolylboronic acid (0.332 g, 2.44 mmol), toluene (10 mL), cesium carbonate (0.795 g, 2.44 mmol), and water (1 mL) under argon was added tetrakis(triphenylphosphine)-palladium(0) (128 mg, 0.111 mmol). The mixture was heated under reflux for 15 h. After cooling, the mixture was filtered through Celite and the filter cake was washed with EtOAc. The filtrate was washed with brine, dried (Na2SO4), and concentrated. The residue was purified by silica gel column (0-100% EtOAc/hexane) to yield a white solid. LC-MS: 3.26 min, 305.3 [M+1]+ (weak).

1. temperatureThe mixture was heated
2. temperatureunder reflux for 15 h
3. temperatureAfter cooling
4. filtrationthe mixture was filtered through Celite
5. washthe filter cake was washed with EtOAc
6. washThe filtrate was washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. customThe residue was purified by silica gel column (0-100% EtOAc/hexane)
10. customto yield a white solid
11. custom3.26 min, 305.3 [M+1]+ (weak)