反应详情

6-Bromo-3-fluoro-4-nitro-1-(phenylsulfonyl)-1H-indazole (5.9 g) was suspended in acetic acid (60 ml) and iron powder (4.12 g) was added. The suspension was heated to reflux. After 2 h the reaction mixture was diluted with ethyl acetate (100 ml) and filtered through celite. The filter cake was washed well with ethyl acetate then the filtrate basified to pH 8-9. The biphasic system was then stirred for ˜5 min. The layers were then separated, the aq washed with ethyl acetate and the combined organics washed with brine, dried (magnesium sulphate), filtered and concentrated in vacuum to yield a crude loaded onto a 330 g silica cartridge, purified on a 0-100% ethyl acetate:cyclohexane gradient and the relevant fractions combined and concentrated to yield the title compound, 2.4 g as a yellow solid.

1. temperatureThe suspension was heated to reflux
2. filtrationfiltered through celite
3. washThe filter cake was washed well with ethyl acetate
4. customThe layers were then separated
5. washthe aq washed with ethyl acetate
6. washthe combined organics washed with brine
7. dry with materialdried (magnesium sulphate)
8. filtrationfiltered
9. concentrationconcentrated in vacuum
10. customto yield a crude
11. custompurified on a 0-100% ethyl acetate
12. concentrationconcentrated