反应详情

温度

130 °C

To a stirred solution of compound (xiii) (4.49 g, 12.86 mmol) in DMF (50 mL) was added sodium cyanide (1.34 g, 27.73 mmol) at RT and the reaction mixture was then heated at 130° C. for 2 h. The reaction mixture was then diluted with saturated FeCl3 solution and extracted with EtOAc (3×75 mL). The combined organic layers were washed with water, dried (Na2SO4) and concentrated to give the crude product which was purified by column chromatography on 100-200 mesh silica gel eluting with EtOAc/hexane (2-4%) to give 6-bromo-2-(4-fluorophenyl)-2H-indazole-3-carbonitrile (xiv) (2.2 g, 50%) as white solid. ESI-MS m/z calculated for [M+H]+: 317.99; found: 317.90.

1. extractionextracted with EtOAc (3×75 mL)
2. washThe combined organic layers were washed with water
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated
5. customto give the crude product which
6. customwas purified by column chromatography on 100-200 mesh silica gel eluting with EtOAc/hexane (2-4%)