反应详情

5m (216 mg, 0.47 mmol) was dissolved in 1,4-dioxane (5 mL) and degassed with N2 for 20 minutes. Potassium tert-butoxide (55 mg, 0.49 mmol) was added, and the reaction was stirred at room temperature overnight. The mixture was degassed with N2 for an additional 20 minutes, and then 4-(3-Bromo-phenyl)-tetrahydro-pyran-4-carboxylic acid methyl ester (5o, 141 mg, 0.47 mmol) in 1,4-dioxane (1 mL) was added, followed by iPr2NEt (0.18 mL, 1.03 mmol), Pd2dba3 (11 mg, 0.01 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (15 mg, 0.02 mmol). The reaction was sealed and heated to 110° C. for 1.5 hours. The mixture was cooled to room temperature and concentrated, and the residue was purified by silica gel chromatography (20-100% EtOAc in hexanes, followed by 0-10% MeOH in EtOAc) to give the desired product, 5p.

1. customdegassed with N2 for 20 minutes
2. customThe mixture was degassed with N2 for an additional 20 minutes
3. customThe reaction was sealed
4. temperatureheated to 110° C. for 1.5 hours
5. temperatureThe mixture was cooled to room temperature
6. concentrationconcentrated
7. customthe residue was purified by silica gel chromatography (20-100% EtOAc in hexanes, followed by 0-10% MeOH in EtOAc)