反应详情

温度

80 °C

1g (230 mg, 0.82 mmol) and 4-(3-Fluoro-5-mercapto-phenyl)-tetrahydro-pyran-4-carbonitrile (1h, 230 mg, 0.99 mmol) were dissolved in 1,4-dioxane (10 mL) and degassed with N2 for 10 minutes. iPr2NEt (0.35 mL, 2.0 mmol), Pd2dba3 (20 mg, 0.02 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (24 mg, 0.04 mmol) were added, and the mixture was degassed with N2 for an additional 10 minutes. The reaction was heated to 80° C. overnight, then cooled to room temperature, concentrated, and purified by silica gel chromatography to give the desired product, 1k.

1. customdegassed with N2 for 10 minutes
2. customthe mixture was degassed with N2 for an additional 10 minutes
3. temperaturecooled to room temperature
4. concentrationconcentrated
5. custompurified by silica gel chromatography