反应详情

温度

105 °C

In a 15 mL microwave reaction vial was added a solution of 5-((cyclobutylamino)methyl)pyrazin-2-amine (280 mg, 1.57 mmol, Eq: 1.00) in dioxane (7 ml) under argon bubbling. To the solution was added 4-bromo-6-chloro-2-methylpyridazin-3(2H)-one (456 mg, 2.04 mmol, Eq: 1.3), Cs2CO3 (1.3 g, 3.99 mmol, Eq: 2.54), xantphos (136 mg, 236 mmol, Eq: 0.15) and bis(dibenzylideneacetone)palladium (67.7 mg, 118 μmol, Eq: 0.075). The reaction tube was sealed and heated in oil bath at 105° C. (bath temp) for 7 hrs then stirred at room temperature overnight. The crude reaction mixture was filtered and the solid was washed with dioxane (20 mL) and DCM (5 mL). The combined filtrate and washes were concentrated and absorbed on silica gel. The mixture was purified by LC chromatography (silica gel, 60 g) and eluted with 0-10% (10% NH4OH in MeOH) in ( 1/1) EtOAc/Heptane to afford 197 mg (39%) of the title compound.

1. customIn a 15 mL microwave reaction
2. customThe reaction tube was sealed
3. customThe crude reaction mixture
4. filtrationwas filtered
5. washthe solid was washed with dioxane (20 mL) and DCM (5 mL)
6. concentrationThe combined filtrate and washes were concentrated
7. customabsorbed on silica gel
8. customThe mixture was purified by LC chromatography (silica gel, 60 g)
9. washeluted with 0-10% (10% NH4OH in MeOH) in ( 1/1) EtOAc/Heptane