反应详情

温度

70 °C

To a solution of 10.0 g of 5-bromo-6-fluoro-1H-indazole in 150 mL of N,N-dimethylformamide was added 10.5 g of N-iodosuccinimide at room temperature, and stirred at 70° C. for 2 days. Then the solution was diluted with ethyl acetate, washed successively with aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crystals precipitated by adding diethyl ether to the residue were collected by filtration. The filtrate was further concentrated and purified and separated by silica gel column chromatographsy (ethyl acetate:n-hexane=1:10-1:5) and combined with the previous crystals, to afford 14.5 g of the title compound as colorless crystals.

1. washwashed successively with aqueous ammonium chloride and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customthe solvent was evaporated
4. customThe crystals precipitated
5. additionby adding diethyl ether to the residue
6. filtrationwere collected by filtration
7. concentrationThe filtrate was further concentrated
8. custompurified
9. customseparated by silica gel column chromatographsy (ethyl acetate:n-hexane=1:10-1:5)