反应详情

温度

95 °C

A mixture of N-(2-Fluoro-4-iodophenyl)methanesulfonamide (13-3, 5 mmol) and palladium(II)acetate (0.15 nM, 0.034 g), 1,3-bisdiphenyl phosphinoprophan (0.3 mM, 0.124 g), thallium(I)acetate (5.5 mM, 1.450 g) and butylvinyl ether (10 mM, 1.3 mL) in DMF (10 mL) was heated at 95° C. for 19 h. The reaction mixture was cooled to room temperature, diluted with THF, treated with 10% HCl (10 mL) and stirred at room temperature. A mixture was diluted with EtOAc, washed with ammonium chloride solution three times and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using EtOAc:hexanes as eluant to 3′-Fluoro-4′-(methylsulfonylamino)acetophenone (13-6, LJO-363).

1. temperatureThe reaction mixture was cooled to room temperature
2. washwashed with ammonium chloride solution three times
3. concentrationconcentrated in vacuo
4. customThe residue was purified by flash column chromatography on silica gel