反应详情

6-Chloro-4-fluoro-1H-indazole (7.6 g, 44.6 mmol) was dissolved in DMF (110 ml). Iodine (22.6 g, 89.1 mmol) was added followed by potassium hydroxide (9.5 g, 169 mmol). The reaction was stirred at room temperature for 1.5 h. Water, 1 M sodium thiosulfate solution and diethyl ether were added. The layers were separated and the aqueous layer was extracted once more with ether. The organic layers were washed with water and sodium chloride solution, and then dried over sodium sulfate. Evaporation of the solvent gave 11.16 g (85%) of 6-chloro-4-fluoro-3-iodo-1H-indazole as a light brown solid (M−H)−=295.

1. customThe layers were separated
2. extractionthe aqueous layer was extracted once more with ether
3. washThe organic layers were washed with water and sodium chloride solution
4. dry with materialdried over sodium sulfate
5. customEvaporation of the solvent