反应详情

5-Cyano-7-iodo-1-phenylbenzimidazole (173 mg, 0.5 mmol), toluene (3.0 ml), tetrakis(triphenylphosphine)palladium(0) (58 mg, 0.05 mmol), 3-acetamidophenylboronic acid (90 mg, 0.5 mmol), ethanol (3.0 ml) and potassium carbonate (138 mg, 1.0 mmol) were combined and the mixture was stirred at reflux overnight. The solvent was removed under reduced pressure and the crude product was purified on a 2 g silica Isolute® SPE column, eluting with dichloromethane/methanol (98:2). The eluent from this column was evaporated under reduced pressure and the crude product was purified further by prep LCMS, then recrystallised from dichloromethane/diethyl ether to give the product as a white solid (64 mg, 36%) m/z, 353.0 (M+H)+.

1. temperatureat reflux overnight
2. customThe solvent was removed under reduced pressure
3. customthe crude product was purified on a 2 g silica Isolute® SPE column
4. washeluting with dichloromethane/methanol (98:2)
5. customThe eluent from this column was evaporated under reduced pressure
6. customthe crude product was purified further by prep LCMS
7. customrecrystallised from dichloromethane/diethyl ether