反应详情

温度

100 °C

To a solution of 6-(1-methyl-1H-pyrazol-4-yl)-[1,2,4]triazolo[4,3-b]pyridazine-3-thiol (2.3 g, 10.0 mmol) in DMF (20 mL) is added 5-iodo-2-methyl-2H-indazole (2.6 g, 10.0 mmol), tris(dibenzylideneacetone) dipalladium(0) (460 mg; 502.7 μmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (580 mg, 1.0 mmol), diisopropylethylamine (4 mL, 22.9 mmol). The mixture is purged with N2 and stirred at 100° C. for 18 h. DMF is removed under vacuum, and the residue is purified by flash column chromatography (Combi-Flash, silica gel) eluting with DCM/methanol (20:1) to give a crude product. The crude product is suspended in 20 mL of DCM to give slurry, and the pure product is collected by filtration to afford the title compound (1.9 g, 52.5%) as a yellow solid. MS (m/z): 363.1 (M+H).

1. customThe mixture is purged with N2
2. customDMF is removed under vacuum
3. customthe residue is purified by flash column chromatography (Combi-Flash, silica gel)
4. washeluting with DCM/methanol (20:1)
5. customto give a crude product
6. customto give slurry
7. filtrationthe pure product is collected by filtration