反应详情

A solution of triethyl phosphonoacetate (3.8 mmol, 1.2 eq) in THF (12 ml) was added dropwise to a suspension of NaH (3.8 mmol, 1.2 eq) in THF (12 ml) at 0° C. and the mixture was stirred for 30 min. 1-(4-Methoxy-2,6-dimethylphenylsulfonyl)piperidine-2-carbaldehyde (3.2 mmol) in THF (6 ml) was then added and the mixture was stirred for a further 30 min. The reaction mixture was warmed to room temperature and stirred for 12 h. Hydrolysis was then carried out with water and the mixture was extracted with ethyl acetate. The organic phase was washed with water (20 ml) and saturated sodium chloride solution (20 ml), dried over sodium sulfate and concentrated. The crude product was purified by column chromatography (5-20% ethyl acetate in hexane). Yield: 40%

1. stirringthe mixture was stirred for a further 30 min
2. stirringstirred for 12 h
3. customHydrolysis
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic phase was washed with water (20 ml) and saturated sodium chloride solution (20 ml)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customThe crude product was purified by column chromatography (5-20% ethyl acetate in hexane)