反应详情

To a suspension of 3-amino-1H-indazole-6-carbonitrile (345 mg) in AcOH was slowly added an aqueous NaNO2 solution (301 mg) at 0° C. It was stirred at room temperature for 2.5 days, and the residue was collected by filtration, and washed with cool water. To the residue were added 0.1 M HCl and DME, followed by stirring at 80° C. for 2 hours. The reaction mixture was neutralized with a saturated aqueous NaHCO3 solution, and extracted with EtOAc. The organic layer was dried over anhydrous MgSO4, and concentrated. The residue was purified by silica gel column chromatography (n-hexane:EtOAc=80:20 to 50:50) to obtain 1H-indazole-6-carbonitrile (175 mg) as a yellow solid.

1. filtrationthe residue was collected by filtration
2. washwashed with cool water
3. additionTo the residue were added 0.1 M HCl and DME
4. stirringby stirring at 80° C. for 2 hours
5. extractionextracted with EtOAc
6. dry with materialThe organic layer was dried over anhydrous MgSO4
7. concentrationconcentrated
8. customThe residue was purified by silica gel column chromatography (n-hexane:EtOAc=80:20 to 50:50)