反应详情

温度

90 °C

5k (201 mg, 0.54 mmol) was suspended in 1,4-dioxane (4.5 mL) and degassed with N2 for 5 minutes. iPr2NEt (0.19 mL, 1.08 mmol) was added, followed by 4-(3-Mercapto-phenyl)-tetrahydro-pyran-4-ol (51, 131 mg, 0.60 mmol) in 1,4-dioxane (1 mL). Pd2dba3 (13 mg, 0.01 mmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (16 mg, 0.03 mmol) were added, and the reaction was sealed and heated to 90° C. overnight. After cooling to room temperature, the mixture was concentrated and purified by silica gel chromatography (20-100% EtOAc in hexanes, followed by 0-10% MeOH in EtOAc) to obtain the desired product, 5p. Further purification by preparative HPLC was required, followed by standard aqueous workup of the combined fractions using EtOAc and saturated aqueous NaHCO3 to give clean product.

1. customdegassed with N2 for 5 minutes
2. customthe reaction was sealed
3. temperatureAfter cooling to room temperature
4. concentrationthe mixture was concentrated
5. custompurified by silica gel chromatography (20-100% EtOAc in hexanes, followed by 0-10% MeOH in EtOAc)