反应详情

温度

110 °C

Palladium (II) acetate (2 mg, 0.01 mmol) was added to a degassed, ambient temperature solution of N-{2-(4-bromophenyl)-1-[1-[(dimethylamino)sulfonyl]-4-(2,2-dimethylbutyl)-1H-imidazol-2-yl]ethyl}acetamide (100 mg, 0.2 mmol), sodium tert-butoxide (77 mg, 0.8 mmol), 1-{[2-(trimethylsilyl)ethoxy]methyl}-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-b]pyridine (102 mg, 0.4 mmol) and 2-(dicyclohexylphosphino)biphenyl (7 mg, 0.02 mmol) in 1,4-dioxane (5 mL). After stirring at 110° C. overnight, the reaction mixture was cooled, diluted with water and extracted with methylene chloride and ethyl acetate. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-60% acetone/methylene chloride afforded N-{1-[1-[(dimethylamino)sulfonyl]-4-(2,2-dimethylbutyl)-1H-imidazol-2-yl]-2-[4-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1,4,5,6-tetrahydro-7H-pyrazolo[3,4-b]pyridin-7-yl)phenyl]ethyl}acetamide.

1. temperaturethe reaction mixture was cooled
2. extractionextracted with methylene chloride and ethyl acetate
3. dry with materialThe combined organic extracts were dried (magnesium sulfate)
4. concentrationconcentrated in vacuo