反应详情

温度

0 °C

A solution of methyl dimethylphosphonoacetate (21.5 g) in N,N-dimethylformamide (50 mL) was added dropwise to a suspension of sodium hydride (63%, 4.50 g) in N,N-dimethylformamide (100 mL) with stirring at 0° C. The mixture was stirred at 0° C. for 30 minutes. Then, a solution of phthalimidoacetone (20.0 g) in N,N-dimethylformamide (50 mL) was added dropwise thereto, and the mixture was heated to room temperature and stirred overnight. To the reaction solution, water was added, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of ammonium chloride and saturated sodium chloride solution and dried over anhydrous sodium sulfate. After filtration and concentration under reduced pressure, the obtained crude product was purified by silica gel column chromatography to obtain the title compound (20.6 g).

1. stirringThe mixture was stirred at 0° C. for 30 minutes
2. temperaturethe mixture was heated to room temperature
3. stirringstirred overnight
4. extractionfollowed by extraction with ethyl acetate
5. washThe organic layer was washed with a saturated aqueous solution of ammonium chloride and saturated sodium chloride solution
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationAfter filtration and concentration under reduced pressure
8. customthe obtained crude product
9. customwas purified by silica gel column chromatography