反应详情

温度

0 °C

1x (200 mg, 0.43 mmol) in 1,4-dioxane (5 mL) was degassed with N2 for 10 minutes and cooled to 0° C. Potassium tert-butoxide (73 mg, 0.65 mmol) was added, and the mixture was stirred at room temperature for 5 minutes. The solution was degassed with N2 for another 5 minutes while 4-(3-bromo-phenyl)-tetrahydro-pyran-4-carboxylic acid methyl ester (1y, 130 mg, 0.43 mmol), Pd2dba3 (10 mg, 0.01 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (11 mg, 0.02 mmol), and iPr2NEt (0.15 mL, 0.87 mmol) were added. The reaction was heated to 60° C. overnight, and then cooled to room temperature and concentrated. The residue was purified by silica gel chromatography (0-100% EtOAc in hexanes) to give the desired product, 1z.

1. additionwere added
2. temperatureThe reaction was heated to 60° C. overnight
3. temperaturecooled to room temperature
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography (0-100% EtOAc in hexanes)