反应详情

温度

80 °C

To a stirred solution of 3-(4-bromo-phenyl)-1-(2-methyl-pyridin-4-yl)-3-o-tolyl-propan-1-one (400 mg), (4-methoxycarbonylphenyl)boronic acid (275 mg), dichlor(1,1′-bis(diphenyl-phosphino)-ferrocene)palladium (II) dichloromethane adduct (41 mg) in dioxane (3 mL) and water (2.6 mL) was added a 2 M aqueous sodium carbonate solution (1.52 mL). The mixture was stirred at 80° C. for 1.5 h. A saturated solution of NH4Cl was added, the phases were separated and the inorganic one was extracted with EtOAc (2×). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by flash chromatography on silica gel (EtOAc/n-heptane 1:1) to yield the title compound as a yellow foam (400 mg, 88%), MS (ESI+): m/z=450.2063 ([M+H]+).

1. customthe phases were separated
2. extractionthe inorganic one was extracted with EtOAc (2×)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by flash chromatography on silica gel (EtOAc/n-heptane 1:1)