反应详情

Stir together 3′-chloro-4-(5-methyl-1-phenyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (184 mg, 0.50 mmol), [2-fluoro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-methanol (151 mg, 0.60 mmol), potassium carbonate (166 mg, 1.20 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.006 g, 0.003 mmol) and water (1 mL), in N,N-dimethylacetamide (2 mL) at room temperature under nitrogen, then heat at 120° C. for 3 hr. Cool to room temperature, add water (20 mL) and extract with DCM (3×20 mL). Pass the combined DCM extracts through an IST Phase Separator Frit®, concentrate and purify (silica gel chromatography, eluting with 5:95 to 15:85 methanol:DCM). Dry in a vacuum oven over night, then dissolve the yellow powder in acetonitrile. Add 2 M aq. HCl and water then lyophilize to give the title compound as light yellow powder (203 mg, 82%). MS (ES): m/z=459 [M+H].

1. extractionextract with DCM (3×20 mL)
2. concentrationconcentrate
3. custompurify
4. wash(silica gel chromatography, eluting with 5:95 to 15:85 methanol:DCM)
5. customDry in a vacuum oven over night
6. dissolutiondissolve the yellow powder in acetonitrile
7. additionAdd 2 M aq. HCl and water