反应详情

温度

110 °C

A mixture of potassium carbonate (3.0 g, 21.9 mmol, 1.1 eq), 3-iodophenol (4.4 g, 19.9 mmol) and 6-(2,4,6-triiodophenoxy)-1-chlorohexane (11.75.g, 19.9 mmol) in 50 ml of DMF was heated to 110° C. for 1.5 hours and then cooled. The mixture was poured into water and extracted with ethyl acetate. The organic layer was dried (magnesium sulfate) and evaporated to give a solid which was filtered through basic alumina (hexanes-ethyl acetate). The filtrate was concentrated under vacuum leaving the crude product as a solid. Recrystallization from cyclohexane afforded 8.29 g (54%) of the desired product after drying at room temperature under high vacuum, mp 65°-66° C.

1. temperaturecooled
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried (magnesium sulfate)
4. customevaporated
5. customto give a solid which
6. filtrationwas filtered through basic alumina (hexanes-ethyl acetate)
7. concentrationThe filtrate was concentrated under vacuum
8. customleaving the crude product as a solid
9. customRecrystallization from cyclohexane