反应详情

A solution of methylmagnesium bromide in THF (0.96 M, 88.1 mL) was added to a solution of 2,6-difluoro-N-methoxy-N-methylnicotinamide (7.01 g) in tetrahydrofuran (180 mL) under ice-cooling, and the reaction solution was stirred under ice-cooling for two hours. A saturated ammonium chloride solution and ethyl acetate were added to the reaction solution under ice-cooling, and the organic layer was separated. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent: hexane-ethyl acetate) to obtain 4.74 g of the title compound.

1. temperaturecooling
2. temperaturecooling for two hours
3. temperaturecooling
4. customthe organic layer was separated
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customthe residue was purified by silica gel column chromatography (elution solvent: hexane-ethyl acetate)