反应详情

温度

60 °C

To a stirred solution of 3,5-bis(trifluoromethyl)phenyl boric acid (20.0 g) in tetrahydrofuran (100 mL) and water (40 mL) was added 2-bromo-3,3,3-trifluoropropene (20.2 g) and potassium carbonate (30.0 g), followed by the addition of 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene(1,4-naphthoquinone)palladium(0) dimer (0.023 g). The reaction mixture was stirred at 60° C. for 3 hours under nitrogen atmosphere and then cooled to room temperature. The resulting mixture was poured into ice-water (100 mL) and extracted with ethyl acetate (100 mL×2). The organic extracts were combined, washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to provide a residue. The residue was purified by column chromatography on silica gel eluted with hexane to afford the title compound as orange oil (21.9 g).

1. temperaturecooled to room temperature
2. extractionextracted with ethyl acetate (100 mL×2)
3. washwashed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customto provide a residue
7. customThe residue was purified by column chromatography on silica gel
8. washeluted with hexane