反应详情

Combine 3′-chloro-4-(5-methyl-1-phenyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.290 g, 0.786 mmol), potassium carbonate (0.261 g, 1.89 mmol), (4-acetamidomethylphenyl)boronic acid (0.182 g, 0.943 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.009 g, 0.008 mmol) in N,N-dimethylacetamide (1.6 mL). Add water (790 μL), and reflux reaction for 18 hr. Add DCM and wash with water. Extract water layer three times with DCM. Dry combined organics (magnesium sulfate) and purify (silica gel chromatography, eluting with 50:50 to 100:0 ethyl acetate:hexanes then 10:90 to 20:80 methanol:ethyl acetate), to give the free base of the title compound (365 mg, 96%). Dissolve the free base (0.363 g, 0.754 mmol) in acetonitrile (904 μL) and add aq. 1 N HCl solution (904 μL, 0.904 mmol). Shake for 15 min. at ambient temperature. Freeze dry to give the title compound (392 mg, 100%). MS (ES): m/z=482 [M+H]+.

1. customreaction for 18 hr
2. washAdd DCM and wash with water
3. customDry
4. custompurify (silica gel chromatography
5. washeluting with 50:50 to 100:0 ethyl acetate