反应详情

A mixture of (4-(N,N-dimethylcarbamoylthio)-2-hydroxy-3-propylphenyl)ethanone (26.6 g), ethyl 4-bromobutyrate (92.9 g), potassium iodide (1 g) and potassium carbonate (26.1 g) in acetone (200 ml) was heated and refluxed with stirring. Each of potassium carbonate (13 g) was added thereto after 9 hours and 14 hours, and the mixture was heated and refluxed with stirring for total 29 hours. Then, inorganic materials were separated and the solution was concentrated under a reduced pressure. The resultant residue was purified through silica-gel column chromatography (eluting with hexane, then benzene and finally benzene:ethyl acetate=9:1) to give ethyl 4-(6-acetyl-3-(N,N-dimethylcarbamoylthio) -2-propylphenoxy)butyrate (31.5 g, 84.2%) as light brown crystal, mp 60-63° C.

1. temperaturewas heated
2. temperaturerefluxed
3. temperature14 hours, and the mixture was heated
4. temperaturerefluxed
5. stirringwith stirring for total 29 hours
6. customThen, inorganic materials were separated
7. concentrationthe solution was concentrated under a reduced pressure
8. customThe resultant residue was purified through silica-gel column chromatography (
9. washeluting with hexane