反应详情

温度

0 °C

To a solution of 6-tert-butyl-3-iodo-1-methyl-1H-indazole (150 mg, 0.45 mmol) in THF (3 mL) at 0° C. was slowly added isopropylmagnesium chloride (2.0 M in THF, 0.27 mL, 0.54 mmol). The bright yellow heterogeneous reaction mixture was stirred at 0° C. for 1 h then tributylchlorostannane (0.15 mL, 0.54 mmol) was added dropwise. Stirring was continued at 0° C. for 20 min then at room temperature for 3 h. The reaction mixture was quenched with water and extracted with EtOAc (2×). The combined organics were washed with brine then dried over MgSO4 and concentrated to afford 6-tert-butyl-1-methyl-3-tributylstannanyl-1H-indazole as a viscous yellow oil which was used in the next step without further purification.

1. customat 0° C.
2. stirringStirring
3. waitwas continued at 0° C. for 20 min
4. waitat room temperature for 3 h
5. customThe reaction mixture was quenched with water
6. extractionextracted with EtOAc (2×)
7. washThe combined organics were washed with brine
8. dry with materialthen dried over MgSO4
9. concentrationconcentrated