反应详情

A solution of DME (40 mL) and 2M K2CO3 (40 mL) containing 1-bromo-3-chlorobenzene (2.53 g, 13.21 mol), 4-(trifluoromethoxy)phenyl boronic acid (4 g, 19.4 mmol) and Pd(PPh3)4 (0.76 g, 0.66 mmol) was refluxed under an argon atmosphere until no starting material remained by HPLC analysis. The solution was concentrated (to remove excess DME) and partitioned between water and ethyl acetate. The organic phase was washed with 1N NaOH, water (2×) and brine. The solution was then dried over MgSO4, filtered and concentrated. The residue was purified by silica gel chromatography using a hexanes/ethyl acetate gradient to give the title compound. LCMS1 4.23 min.

1. temperaturewas refluxed under an argon atmosphere until no starting material
2. concentrationThe solution was concentrated
3. custom(to remove excess DME)
4. custompartitioned between water and ethyl acetate
5. washThe organic phase was washed with 1N NaOH, water (2×) and brine
6. dry with materialThe solution was then dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified by silica gel chromatography