反应详情

温度

120 °C

2′,4,6′-trifluorobiphenyl-3-carbaldehyde (160 g, 695.01 mmol) was taken in hydrazine hydrate (800 mL) and heated to 120° C. for 8 h. The reaction mixture was cooled to RT. Water was added to the reaction mixture and extracted with EtOAc (2×500 mL). Organic layer was washed with brine and dried over Na2SO4. The organic layer was concentrated and purified by column using silica (100-200 mesh) and 0-15% EtOAc-hexane to provide 5-(2,6-difluoro-phenyl)-1H-indazole (40.8 g, 25.4% yield). MS (ESI, pos. ion) m/z: 231.1 (M+1).

1. temperatureThe reaction mixture was cooled to RT
2. extractionextracted with EtOAc (2×500 mL)
3. washOrganic layer was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationThe organic layer was concentrated
6. custompurified by column