反应详情

温度

95 °C

A mixture of compound (xii) (6.44 g, 19.20 mmol) and POCl3 (50 mL) was heated at 95° C. for 6 h. The volatiles were removed under reduced pressure and the residue was basified by the addition of an ice-cold saturated solution of sodium carbonate. The solid obtained was filtered and dried (Na2SO4) to give the crude product which was purified by column chromatography on 100-200 mesh silica gel eluting with EtOAc/hexane (3-5%) to give 6-bromo-3-chloro-2-(4-fluorophenyl)-2H-indazole (xiii) (4 g, 64%) as a white solid. ESI-MS m/z calculated for [M+H]+: 326.95; found: 326.95.

1. customThe volatiles were removed under reduced pressure
2. additionthe residue was basified by the addition of an ice-cold saturated solution of sodium carbonate
3. customThe solid obtained
4. filtrationwas filtered
5. dry with materialdried (Na2SO4)
6. customto give the crude product which
7. customwas purified by column chromatography on 100-200 mesh silica gel eluting with EtOAc/hexane (3-5%)