反应详情

温度

-16 °C

5-(Difluoromethoxy)-3-iodo-1-methyl-1H-indazole (0.265 g, 818 μmol) was dissolved in THF (3.00 mL). The colorless solution was cooled to −16° C. (NaCl/ice bath) then isopropylmagnesium chloride (2M in THF, 458 μL, 916 μmol) added dropwise at −16° C. The reaction mixture was stirred at −16° C. for 20 min then tributylchlorostannane (306 mg, 255 μL, 940 μmol) was added slowly. The reaction mixture was warmed to 25° C. and stirred for 1.5 h. The reaction mixture was quenched with saturated ammonium chloride solution, extracted with dichloromethane (3×30 mL), organics dried over MgSO4 and concentrated to a yellow oil. The residue was dried under high vacuum and taken into next step without further purification.

1. temperatureThe reaction mixture was warmed to 25° C.
2. stirringstirred for 1.5 h
3. customThe reaction mixture was quenched with saturated ammonium chloride solution
4. extractionextracted with dichloromethane (3×30 mL)
5. dry with materialorganics dried over MgSO4
6. concentrationconcentrated to a yellow oil
7. customThe residue was dried under high vacuum
8. customtaken into next step without further purification