反应详情

温度

80 °C

To a microwave vial was added 3-chloro-2-phenyl-9-pyrazin-2-yl[1,2,4]triazolo[4′,3′:1,6]pyrido[2,3-b]pyrazine (8-5, 0.151 g, 0.421 mmol), tert-butyl {1-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]cyclobutyl}carbamate (8-6, 0.236 g, 0.631 mmol), potassium carbonate (0.174 g, 1.262 mmol), bis(tri-t-butylphosphine)palladium(0) (21.51 mg, 0.042 mmol), water (0.2 mL), NMP (0.2 mL), and 1,4 Dioxane (0.8 mL). The reaction mixture was then heated to 80° C. under microwave irradiation for 10 minutes. The reaction mixture was then permitted to cool to room temperature, diluted with NMP/MeOH, and filtered through a syringe filter. The resulting residue was then purified by reverse phase column chromatography (Sunfire C18) eluting with 5 to 100% acetonitrile/(0.1% TFA/water) gradient. The appropriate fractions were then concentrated in vacuo to give 8-7 as a green solid. HRMS (M+H)+: observed=571.2591, calculated=571.2565.

1. temperatureto cool to room temperature
2. filtrationfiltered through a syringe
3. filtrationfilter
4. customThe resulting residue was then purified by reverse phase column chromatography (Sunfire C18)
5. washeluting with 5 to 100% acetonitrile/(0.1% TFA/water) gradient
6. concentrationThe appropriate fractions were then concentrated in vacuo