Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-Iodophenol | HCID 12272 | — |
| Edukt | 6-(2,4,6-Triiodophenoxy)-1-chlorohexane | HCID 15224801 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 1-(3-Iodophenoxy)-6-(2,4,6-triiodophenoxy)-hexane | HCID 15224802 | 54% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US05492687 |
|---|
| Quelldatensatz | uspto-grants-1996_02 |
|---|
| ORD ID | ord-6abb4f83bc43455e97a87675cd7e5c5e |
|---|
| Quellennotiz | uspto-grants-1996_02 |
|---|