反应详情

To a mixture of 4′-[(6-ethyl-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl)methyl]biphenyl-2-carbonitrile (1.0 g), 2-bromo-1-pyridin-4-yl-ethanone hydrogen bromide (1.09 g) and N,N-dimethylformamide (8 mL) was added 60% sodium hydride (0.31 g), and the mixture was stirred at room temperature for 20 hr. After allowing to cool to room temperature, ethyl acetate and water were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was successively washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a pale-yellow amorphous solid (0.20 g, 15%).

1. temperatureto cool to room temperature
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was successively washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography