反应详情

Combine 3′-chloro-4-(1-ethyl-5-methyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.300 g, 0.935 mmol), potassium carbonate (0.310 g, 2.24 mmol), (4-acetamidomethylphenyl)boronic acid (0.216 g, 1.12 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.011 g, 0.009 mmol) in N,N-dimethylacetamide (1.9 mL). Add water (940 μL), and reflux reaction for 6 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 (384 mg, 95%). Dissolve the free base (0.381 g, 0.880 mmol) in acetonitrile (1.06 mL) and add aq. 1 N HCl solution (1.06 mL, 1.06 mmol). Shake for 15 min. at ambient temperature. Freeze dry to give the title compound (416 mg, 100%). MS (ES): m/z=434 [M+H]+.

1. customreaction for 6 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