反应详情

温度

-16 °C

In a round-bottomed flask, 3-iodo-6-methanesulfonyl-1-methyl-1H-indazole (120 mg, 0.36 mmol) was dissolved in THF (2 ml). The colorless solution was cooled to −16° C. (NaCl/ice bath) and isopropylmagnesium chloride (2.0 M in THF, 0.25 ml, 0.50 mmol) was added dropwise. The reaction mixture was stirred at −16° C. for 1 h then tributylchlorostannane (0.12 ml, 0.44 mmol) was slowly added. The reaction mixture was allowed to warm to room temperature over 2.5 h then quenched with saturated NH4Cl-solution and extracted with EtOAc (2×). The combined organic layers were washed with water and brine then dried over sodium sulfate, filtered and concentrated to afford 6-methanesulfonyl-1-methyl-3-tributylstannanyl-1H-indazole as a light yellow oil which was used without further purification.

1. additionwas added dropwise
2. temperatureto warm to room temperature over 2.5 h
3. customthen quenched with saturated NH4Cl-solution
4. extractionextracted with EtOAc (2×)
5. washThe combined organic layers were washed with water and brine
6. dry with materialthen dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated