反应详情

温度

130 °C

9d (233 mg, 0.88 mmol) and 3-mercaptopropionic acid 2-ethylhexyl ester (86 mg, 0.38 mmol) were dissolved in 1,4-dioxane (10 mL) and degassed with N2 for 10 minutes. iPr2NEt (0.33 mL, 1.80 mmol) was added, followed by Pd2dba3 (20 mg, 0.02 mmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (23 mg, 0.04 mmol). The reaction was sealed and heated overnight at 130° C., and then cooled to room temperature and diluted with EtOAc and water. The organic layer was washed with water and brine, dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (0-20% MeOH in EtOAc) to give the desired product, 9e.

1. customdegassed with N2 for 10 minutes
2. customThe reaction was sealed
3. temperaturecooled to room temperature
4. washThe organic layer was washed with water and brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica gel chromatography (0-20% MeOH in EtOAc)