反应详情

A mixture of ethyl 4-(6-acetyl-3-mercapto-2-propylphenoxy)-butyrate (1.7 g), (4-(3-bromopropoxy)-2-hydroxy-3-propylphenyl)-ethanone (1.7 g), potassium iodide (0.5 g) and potassium carbonate (1.45 g) in acetone (40 ml) was heated with refluxing and stirring for 7.5 hours. Ice-water and conc. hydrochloric acid were added thereto, and the mixture was subjected to extraction with ethyl acetate. After washed with water, the extract was dried over sodium sulfate and concentrated under a reduced pressure. The resultant residue was separated and purified through silica-gel column chromatography (eluting with benzene:ethyl acetate=9:1) to give the title compound (2.08 g, 71.0%) as light yellow crystal, mp 87-88° C.

1. temperaturewas heated
2. temperaturewith refluxing
3. extractionthe mixture was subjected to extraction with ethyl acetate
4. washAfter washed with water
5. dry with materialthe extract was dried over sodium sulfate
6. concentrationconcentrated under a reduced pressure
7. customThe resultant residue was separated
8. custompurified through silica-gel column chromatography (eluting with benzene:ethyl acetate=9:1)