反应详情

温度

80 °C

2a (175 mg, 0.59 mmol) and 4-(3-mercapto-phenyl)-tetrahydro-pyran-4-ol (2b, 150 mg, 0.71 mmol) were combined in 1,4-dioxane (6 mL) and degassed with N2 for 10 minutes. iPr2NEt (0.33 mL, 1.8 mmol) was added, followed by Pd2dba3 (14 mg, 0.02 mmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (16 mg, 0.03 mmol). The mixture was degassed with N2 for an additional 10 minutes, and then heated to 80° C. for 24 hours. The reaction was cooled to room temperature, concentrated, and purified by silica gel chromatography (0-20% MeOH in EtOAc) to give the desired product, 2c.

1. customdegassed with N2 for 10 minutes
2. customThe mixture was degassed with N2 for an additional 10 minutes
3. temperatureThe reaction was cooled to room temperature
4. concentrationconcentrated
5. custompurified by silica gel chromatography (0-20% MeOH in EtOAc)