反应详情

温度

80 °C

6-Iodo-1H-quinolin-2-one (5.13 g, 18.9 mmol) and 4-(3-Mercapto-phenyl)-tetrahydro-pyran-4-carbonitrile (5f, 4.57 g, 20.8 mmol) were dissolved in 1,4-dioxane (160 mL) and degassed for 10 minutes with N2. iPr2NEt (6.6 mL, 37.9 mmol) was added, followed by Pd2dba3 (434 mg, 0.47 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (548 mg, 0.95 mmol), and the reaction was degassed for another 10 minutes with N2. The reaction was then sealed and heated to 80° C. overnight. After cooling to room temperature, the reaction was filtered and concentrated, and the residue was purified by silica gel chromatography (0-100% MeOH in EtOAc) to give the desired product, 5g.

1. customdegassed for 10 minutes with N2
2. customthe reaction was degassed for another 10 minutes with N2
3. customThe reaction was then sealed
4. temperatureAfter cooling to room temperature
5. filtrationthe reaction was filtered
6. concentrationconcentrated
7. customthe residue was purified by silica gel chromatography (0-100% MeOH in EtOAc)