HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → Ethyl 2,2-Bis-(3-iodophenoxy)acetate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-Iodophenol | HCID 12272 | — |
| Edukt | Diethyl bromomalonate | HCID 69637 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Ethyl 2,2-Bis-(3-iodophenoxy)acetate | HCID 19959850 | 17,2% |
Reaktionsschritte
A stirred solution of 40.0 g (0.18 mol) of 3-iodophenol, 33.6 ml (0.18 mol) of diethyl bromomalonate and 27.63 g (0.2 moles) of milled anhydrous potassium carbonate in 250 ml dry N,N-dimethylformamide was heated at 110°-120° C. under argon for 14 hours. The mixture was cooled and concentrated in vacuo. The resulting residue was combined with 600 ml of ice-cold water and the oily product was extracted with ethyl acetate (4×150 ml). The combined ethyl acetate extracts were dried (MgSO4) and concentrated in vacuo to an orange oil. The orange oil was purified by chromatography (eluted by 5% methylene chloride in hexanes to 50% methylene chloride in hexanes) to yield 8.1 g (8.5%) of the desired product as a tan oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05620677 |
| Quelldatensatz | uspto-grants-1997_04 |
| ORD ID | ord-aba6f21e242c4e97988ea0ec9c79dcb5 |
| Quellennotiz | uspto-grants-1997_04 |