反应详情

To a stirring suspension of sodium hydride (60% in mineral oil) (0.677 g) in THF (25 ml) at 0° C. was added a solution of 6-bromo-3-fluoro-4-nitro-1H-indazole (4 g) in THF (25 ml) dropwise. The reaction mixture was allowed to stir for 30 min then allowed to warm to RT before benzenesulfonyl chloride (2.17 ml) was added. After approximately two hours the reaction mixture was partitioned between ethyl acetate and water. The layers were separated and the aq was then extracted again with ethyl acetate. The combined organics were then washed with brine, dried over magnesium sulphate, filtered and concentrated. The solid was triturated with methanol (50 ml) and filtered to yield the title compound, 5.96 g as a yellow solid.

1. additionwas added
2. customAfter approximately two hours the reaction mixture was partitioned between ethyl acetate and water
3. customThe layers were separated
4. extractionthe aq was then extracted again with ethyl acetate
5. washThe combined organics were then washed with brine
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe solid was triturated with methanol (50 ml)
10. filtrationfiltered