反应详情

To a stirred solution containing mainly 5-isopropyl-1H-indazole (0.85 g, crude) in 70 mL of DMSO was added KOH (0.52 g, 8 mmol) at room temperature. Then I2 (1.35 g, 5.3 mmol) was added slowly, after the addition, the mixture was stirred at room temperature for 2 hours. The mixture was poured into 200 mL of saturated Na2SO3 solution, then extracted with ethyl acetate (2×100 mL). The combined organic layers was washed with water (100 mL) and brine (100 mL) dried over Na2SO4 and concentrated under reduced pressure to give crude 3-iodo-5-isopropyl-1H-indazole (0.78 g). LCMS: (M+H)+=287.

1. additionafter the addition
2. extractionextracted with ethyl acetate (2×100 mL)
3. washThe combined organic layers was washed with water (100 mL) and brine (100 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure