反应详情

温度

120 °C

A solution of 2-(2-fluoro-5-methylphenyl)pyridin-4-amine (42.5 mg, 0.210 mmol), tert-butyl 4-(7-iodo-2H-pyrazolo[4,3-b]pyridin-2-yl)piperidine-1-carboxylate (60 mg, 0.140 mmol) and t-butoxide (18.85 mg, 0.196 mmol) in xylene (3 mL) was sparged with N2 and then 2-dicyclohexylphosphino-2′,4′,6′-tri-iso-propyl-1,1′-biphenyl (13.36 mg, 0.028 mmol) and tris(dibenzylideneacetone)dipalladium(0) (12.83 mg, 0.014 mmol) were added and the mixture was heated at 120° C. overnight. The reaction was cooled, concentrated, the residue treated with dichloromethane/TFA (1/1) and the solvent was removed in vacuo. The residue was dissolved with methanol and purified with 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)-2-(piperidin-4-yl)-2H-pyrazolo[4,3-b]pyridin-7-amine (49 mg, 87%)

1. temperatureThe reaction was cooled
2. concentrationconcentrated
3. additionthe residue treated with dichloromethane/TFA (1/1)
4. customthe solvent was removed in vacuo
5. dissolutionThe residue was dissolved with methanol
6. custompurified with preparative HPLC
7. washeluting with a gradient of 15-40% acetonitrile (containing 0.035% TFA) in water (containing 0.05% TFA)