反应详情

温度

-10 °C

To a solution of 5,6-dichloro-3-iodo-1-methyl-1H-indazole (150 mg, 0.44 mmol) in THF (3 mL) at −10° C. (ice/acetone) was slowly added isopropylmagnesium chloride (2.0 M in THF, 0.26 mL, 0.52 mmol). The bright yellow heterogeneous reaction mixture was stirred at −10° C. for 15 min then tributylchlorostannane (0.14 mL, 0.52 mmol) was added dropwise. Stirring was continued at −10° C. for 30 min then at room temperature for 1 h. The reaction mixture was quenched with water and extracted with EtOAc (2×). The combined organics were dried over MgSO4 and concentrated to afford 5,6-dichloro-1-methyl-3-tributylstannanyl-1H-indazole as a pale yellow oil which was used in the next step without further purification.

1. customat −10° C.
2. stirringStirring
3. waitwas continued at −10° C. for 30 min
4. waitat room temperature for 1 h
5. customThe reaction mixture was quenched with water
6. extractionextracted with EtOAc (2×)
7. dry with materialThe combined organics were dried over MgSO4
8. concentrationconcentrated