反应详情

NaH (440 mg) was added to a solution of 2-oxopiperidine (1.0 g) in DMF (20 ml) and the mixture was stirred at room temperature for 30 minutes. This solution was added in a single portion to a solution of 2,3-dichloro-1,4-dihydro-1,4-dioxonaphthalene (6.9 g) in DMF (150 ml) and the mixture was stirred at room temperature for 17 hours. The reaction solution was poured into saturated aqueous ammonia and the resulting precipitate was removed by filtration and then the filtrate was extracted with ethyl acetate. The organic layer was washed with water and brine and then dried over anhydrous sodium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography (elution with ethyl acetate-hexane 1:10 solution) to give 2-chloro-1,4-dihydro-1,4-dioxo-3-(2-oxopiperidino)naphthalene (0.49 g) as a light brown powder.

1. stirringthe mixture was stirred at room temperature for 17 hours
2. customthe resulting precipitate was removed by filtration
3. extractionthe filtrate was extracted with ethyl acetate
4. washThe organic layer was washed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was evaporated
7. customthe residue was purified by silica gel column chromatography (elution with ethyl acetate-hexane 1:10 solution)