反应详情

温度

110 °C

8b (66 mg, 0.25 mmol) and 4-(3-Mercapto-phenyl)-tetrahydro-pyran-4-carbonitrile (8c, 90 mg, 0.32 mmol) were dissolved in 1,4-dioxane (5 mL) and degassed for 10 minutes with N2. iPr2NEt (0.15 mL, 0.80 mmol) was added, followed by Pd2dba3 (10 mg, 0.01 mmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (12 mg, 0.02 mmol), and the mixture was degassed with N2 for an additional 10 minutes. The reaction was sealed and heated overnight at 110° C. Additional catalyst was added after 24 hours to push the reaction to completion, and the mixture was heated at 110° C. for another 2 hours. The reaction was cooled to room temperature and purified by silica gel chromatography (25-100% EtOAc in hexanes) to give the desired product, 8d.

1. customdegassed for 10 minutes with N2
2. customthe mixture was degassed with N2 for an additional 10 minutes
3. customThe reaction was sealed
4. additionAdditional catalyst was added after 24 hours
5. customthe reaction to completion
6. temperaturethe mixture was heated at 110° C. for another 2 hours
7. temperatureThe reaction was cooled to room temperature
8. custompurified by silica gel chromatography (25-100% EtOAc in hexanes)