反应详情

To a solution of 3-iodo-5-(trifluoromethyl)-1H-indazole (4.0 g, 12.8 mmol) in THF (80 mL) was added t-BuOK (2.0 g, 17.9 mmol) slowly at 0° C. and mixture stirred for 30 minutes, iodomethane (1.1 mL, 17.9 mmol) was added at 0° C., then warmed to room temperature and stirred for 1.5 hours, quenched with water (30 mL) and extracted with EtOAc (3×30 mL), the organic layer was dried over Na2SO4 and concentrated under reduced pressure. The crude product was washed with ether (5 mL) and filtered to give 3-iodo-1-methyl-5-(trifluoromethyl)-1H-indazole (3.3 g, 79.3%) as a white solid. LCMS: (M+H)+=327.

1. stirringstirred for 1.5 hours
2. customquenched with water (30 mL)
3. extractionextracted with EtOAc (3×30 mL)
4. dry with materialthe organic layer was dried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. washThe crude product was washed with ether (5 mL)
7. filtrationfiltered