反应详情

温度

80 °C

To a solution of sodium hydrogenecarbonate (2.8 g, 34 mmol) in water (70 mL) was added a solution of 6-acetyl-2-bromo-4-chloro-3-methylphenyl trifluoromethanesulfonate (6.7 g, 17 mmol) in toluene (70 mL) followed by (3,5-difluorophenyl)boronic acid (2.9 g, 19 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.98 g, 0.85 mmol). The mixture was bubbled with N2 for 5 min and then heated at 80° C. overnight. The reaction was diluted with water and extracted with ethyl acetate. The combined organic layers were dried, filtered, concentrated and purified on silica gel (eluting with 0-15% of ethyl acetate in hexanes) to give the desired product (5.6 g). LCMS calculated for C15H11BrClF2O (M+H)+: m/z=359.0. found: 359.0.

1. customThe mixture was bubbled with N2 for 5 min
2. additionThe reaction was diluted with water
3. extractionextracted with ethyl acetate
4. customThe combined organic layers were dried
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified on silica gel (eluting with 0-15% of ethyl acetate in hexanes)