反应详情

温度

-20 °C

The solution of 5-(tert-butyldimethylsilyloxy)-3-iodo-1-methyl-1H-indazole (3.8 g, 10 mmol) in 30 mL of dry THF was cooled to −20° C. under nitrogen, isopropylmagnesium chloride (6 mL, 12 mmol, 2M in THF) was added and stirred for 15 min at −20° C. Tributylchlorostannane (12 mL, 14 mmol) was added and the reaction mixture was allowed to warm to room temperature and stirred for 1 h. The mixture was quenched with saturated solution of ammonium chloride, extracted with ethyl acetate (3×50 mL), dried over sodium sulfate and concentrated to give 5-(tert-butyldimethylsilyloxy)-1-methyl-3-(tributylstannyl)-1H-indazole (5.2 g, crude) as a colourless oil, which was used directly in the next step without further purification.

1. temperatureto warm to room temperature
2. stirringstirred for 1 h
3. customThe mixture was quenched with saturated solution of ammonium chloride
4. extractionextracted with ethyl acetate (3×50 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated