反应 #62407

反应方程式

5-bromo-6-fluoro-1H-indazole

N-iodosuccinimide

→

title compound

收率 91.5%

5-Bromo-6-fluoro-3-iodo-1H-indazole

收率 91.5%

溶剂

ethyl acetate

N,N-dimethylformamide

反应条件

后处理

1. 1
   洗涤washed successively with aqueous ammonium chloride and saturated brine
2. 2
   干燥dried over anhydrous magnesium sulfate
3. 3
   其他the solvent was evaporated
4. 4
   其他The crystals precipitated
5. 5
   workup.ADDITIONby adding diethyl ether to the residue
6. 6
   过滤were collected by filtration
7. 7
   浓缩The filtrate was further concentrated
8. 8
   其他purified
9. 9
   其他separated by silica gel column chromatographsy (ethyl acetate:n-hexane=1:10-1:5)

实验过程

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.

来源