反应详情

温度

80 °C

A mixture of 6-bromo-5-hydroxy-1H-indazole (7.0 g, 33.0 mmol), 3,4-difluoronitrobenzene (4.98 mg, 31.0 mmol), NaHCO3 (2.5 g, 31.0 mmol) in DMF (100 mL) is stirred at 80° C. for 4 hours. Then LiCl (10% aqueous solution) is added and the solution is extracted with EtOAc. The organic phase is dried over anhydrous MgSO4, filtered and concentrated. The residue is purified by silica gel column chromatography eluting with PE:DCM (1:1) to give the desired product (5.5 g, 46.6% yield). MS (m/z): 354.0 (M+H).

1. extractionthe solution is extracted with EtOAc
2. dry with materialThe organic phase is dried over anhydrous MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue is purified by silica gel column chromatography
6. washeluting with PE