反应详情

To a solution of 3-Bromo-4-[(2,4-difluorobenzyl)oxy]-1-{[5-(hydroxymethyl)pyrazin-2-yl]methyl}-6-methylpyridin-2(1H)-one (0.35 g, 0.00078 mol) in DMF at 0° C., was added NaH (0.022 g, 0.00092 mol) and stirred for 10 min. Iodomethane (0.05 mL) was added to the reaction and the mixture was stirred at 10° C. for 3 h. DMF was distilled in vacuo and the residue was partitioned between 5% citric acid and EtOAc (15.0 mL). The organic phase was washed with water, dried (Na2SO4) and concentrated to dryness. The residue was purified by flash chromatography (EtOAc), and the appropriate fractions were combined and concentrated to a pale yellow powder.

1. stirringthe mixture was stirred at 10° C. for 3 h
2. distillationDMF was distilled in vacuo
3. customthe residue was partitioned between 5% citric acid and EtOAc (15.0 mL)
4. washThe organic phase was washed with water
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated to dryness
7. customThe residue was purified by flash chromatography (EtOAc)
8. concentrationconcentrated to a pale yellow powder