反应详情

To a solution of methyl 5-(4-fluorophenyl)-6-oxo-1-(3-oxobutan-2-yl)-1,6-dihydropyridine-3-carboxylate (11.1 g, 35.0 mmol) in tetrahydrofuran (175 mL) at 0° C. was added methylmagnesium bromide (3.0 M in THF; 14.0 mL, 42.0 mmol). After 20 min, the mixture was quenched with saturated aqueous sodium bicarbonate. The mixture was cooled to ambient temperature and extracted with ethyl acetate (3×). The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane→80% dichloromethane/ethyl acetate) gave the title compound. MS 334.2 (M+1).

1. customthe mixture was quenched with saturated aqueous sodium bicarbonate
2. extractionextracted with ethyl acetate (3×)
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by silica gel chromatography (100% dichloromethane→80% dichloromethane/ethyl acetate)