反应详情

温度

90 °C

A suspension of 1-((5-fluoropyridin-2-yl)methyl)-3-iodo-4-nitro-1H-indazole (0.968 g, 2.43 mmol) in 4:1 IPA/THF (10 mL) was degassed under argon. To the suspension was added TEA (0.678 mL, 4.86 mmol), potassium trifluoro(vinyl)borate (0.651 g, 4.86 mmol) and PdCl2(dppf)*dcm (0.199 g, 0.243 mmol). The mixture was then heated with stirring at 90° C. for 16 hours under argon. The mixture was allowed to cool, filtered through GF/F paper and concentrated under reduced pressure. The residue was dissolved in DCM and purified by chromatography on silica using a Biotage system, eluting with 1-10% Et2O in DCM. This gave 1-((5-fluoropyridin-2-yl)methyl)-4-nitro-3-vinyl-1H-indazole (229 mg).

1. customwas degassed under argon
2. temperatureThe mixture was then heated
3. temperatureto cool
4. filtrationfiltered through GF/F paper
5. concentrationconcentrated under reduced pressure
6. dissolutionThe residue was dissolved in DCM
7. custompurified by chromatography on silica using a Biotage system
8. washeluting with 1-10% Et2O in DCM