反应详情

To a chilled (−78° C.) solution of 5-bromo-3-methyl-2-methoxypyridine (1.56 mmol) in 2 mL THF was added dropwise n-butyllithium (1.71 mmol from a 2.5 M solution in hexanes). The mixture was stirred for 30 minutes and then 2,2,2-trifluoro-1-[1-(4-fluorophenyl)-1H-indazol-5-yl]ethanone (1.39 mmol) in 3 mL THF was added. After 30 minutes, the mixture was diluted with ether and quenched with aqueous ammonium chloride. The organic layer was washed with brine and dried over magnesium sulfate. Removal of the volatiles in vacuo provided a residue which was purified by Combiflash chromatography using ethyl acetate-hexane. The product-rich fractions were concentrated in vacuo to provide the title compound.

1. waitAfter 30 minutes
2. customquenched with aqueous ammonium chloride
3. washThe organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. customRemoval of the volatiles in vacuo
6. customprovided a residue which
7. customwas purified by Combiflash chromatography
8. concentrationThe product-rich fractions were concentrated in vacuo