反应详情

温度

-16 °C

To a stirred solution of 3-iodo-5-isopropyl-1-methyl-1H-indazole (0.3 g, crude) in 100 mL of dry THF at −16° C. under nitrogen was added i-PrMgCl (0.69 mL, 1.38 mmol, 2M in THF) drop-wise. Then the mixture was stirred at −16° C. for 20 minutes. Tributylchlorostannane (0.39 g, 1.2 mmol) was added slowly and the mixture was stirred at room temperature for 2.5 hours. The solution was quenched by 40 mL of water, extracted with ethyl acetate (2×100 mL), washed with water (2×50 mL), brine (50 mL) and dried over anhydrous sodium sulfate. The drying agent was removed by filtration and the filtrate was evaporated under reduced pressure to give crude 5-isopropyl-1-methyl-3-(tributylstannyl)-1H-indazole as an oil, which was used into next step without further purification.

1. stirringthe mixture was stirred at room temperature for 2.5 hours
2. customThe solution was quenched by 40 mL of water
3. extractionextracted with ethyl acetate (2×100 mL)
4. washwashed with water (2×50 mL), brine (50 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. customThe drying agent was removed by filtration
7. customthe filtrate was evaporated under reduced pressure