反应详情

温度

110 °C

8b (120 mg, 0.48 mmol) and 3-mercaptopropionic acid 2-ethylhexyl ester (110 mg, 0.55 mmol) were dissolved in 1,4-dioxane (5 mL) and degassed for 10 minutes with N2. iPr2NEt (0.16 mL, 0.89 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 at 110° C. for 4 hours. The reaction was cooled to room temperature and purified by silica gel chromatography (25-100% EtOAc in hexanes) to give the desired product, 8e.

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. temperatureThe reaction was cooled to room temperature
5. custompurified by silica gel chromatography (25-100% EtOAc in hexanes)