反应详情

温度

80 °C

A suspension of 5-fluoro-3-methyl-benzo[b]thiophene-2-sulfonic acid(4-bromo-2-trifluoromethyl-phenyl)-amide (0.5 g) and 4-pyridineboronic acid (0.197 g) in 1,2-dimethoxyethane (6 ml), ethanol (2 ml) and 2 M aqueous sodium carbonate solution (4.0 ml) was degassed 3-4 times to remove oxygen, then tetrakis(triphenylphosphine)palladium (0.065 g) was added. The reaction mixture was stirred at 80° C. for 3 h, quenched with ice/water, and extracted with ethyl acetate. The organic layers were washed, dried and concentrated. The residue was chromatographed over silica gel using heptane/ethyl acetate as eluent to obtain the title compound (0.35 g) as a yellowish solid. MS (ISP): 467.3 (M+H)+

1. customwas degassed 3-4 times
2. customto remove oxygen
3. additiontetrakis(triphenylphosphine)palladium (0.065 g) was added
4. customquenched with ice/water
5. extractionextracted with ethyl acetate
6. washThe organic layers were washed
7. customdried
8. concentrationconcentrated
9. customThe residue was chromatographed over silica gel