反应详情

温度

120 °C

tert-Butyl 4-(7-iodo-1H-pyrazolo[4,3-b]pyridin-1-yl)piperidine-1-carboxylate (57.0 mg, 0.067 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (41.4 mg, 0.067 mmol), 2-(2-fluoro-5-methylphenyl)pyridin-4-amine (40.4 mg, 0.200 mmol) and t-butoxide (17.91 mg, 0.186 mmol) were dissolved in dioxane (3 mL) and sparged with N2. Palladium(II) acetate (29.9 mg, 0.133 mmol) and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (41.4 mg, 0.067 mmol) were added next and the mixture was heated at 120° C. for 2 hours. The reaction was cooled to room temperature and diluted with methanol. This mixture was filtered and the filtrate was purified by preparative HPLC using a Sunfire Prep 5 μm C18, 75×30 mm column eluting with a gradient of 15-40% acetonitrile (containing 0.035% TFA) in water (containing 0.05% TFA) to give N-(2-(2-fluoro-5-methylphenyl)pyridin-4-yl)-1-(piperidin-4-yl)-1H-pyrazolo[4,3-b]pyridin-7-amine (17 mg, 32%)

1. customsparged with N2
2. temperatureThe reaction was cooled to room temperature
3. filtrationThis mixture was filtered
4. customthe filtrate was purified by preparative HPLC
5. washeluting with a gradient of 15-40% acetonitrile (containing 0.035% TFA) in water (containing 0.05% TFA)