反应详情

温度

80 °C

4d (80 mg, 0.3 mmol) and 4-(3-Fluoro-5-mercapto-phenyl)-tetrahydro-pyran-4-carbonitrile (4e, 88 mg, 0.37 mmol) were dissolved in 1,4-dioxane (3 mL) and degassed for 10 minutes with N2. iPr2NEt (0.10 mL, 0.6 mmol), Pd2dba3 (14 mg, 0.02 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (17 mg, 0.03 mmol) were added, 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 concentrated and purified by silica gel chromatography (0-20% MeOH in EtOAc) to give the desired product, 4f.

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. concentrationthe reaction was concentrated
6. custompurified by silica gel chromatography (0-20% MeOH in EtOAc)