反应详情

温度

80 °C

At room temperature, 7.2 ml of an aqueous 2M sodium carbonate solution and 167 mg (0.144 mmol) of tetrakis(triphenylphosphine)palladium are added to 1.00 g (2.88 mmol) of the compound from Example 5A and 677 mg (4.33 mmol) of (3-chlorophenyl)boronic acid in 40 ml of DME, and the mixture is subsequently stirred at 80° C. overnight. A saturated aqueous ammonium chloride solution is added, and the reaction mixture is subsequently extracted with dichloromethane. The organic phase is dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient). 173 mg (17% of theory) of the title compound are obtained.

1. extractionthe reaction mixture is subsequently extracted with dichloromethane
2. dry with materialThe organic phase is dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient)