HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2,6-Dimethyl-3-(2,2,2-trifluoroethoxy)pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 2,6-Dimethyl-3-pyridinol | HCID 70732 | — |
| Edukt | 2,2,2-Trifluoroethyl trifluoromethanesulfonate | HCID 80366 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2,6-Dimethyl-3-(2,2,2-trifluoroethoxy)pyridine | HCID 67290268 | 98,7% |
Reaktionsschritte
To a suspension of 2,6-dimethylpyridin-3-ol (5.0 g, 41 mmol) and cesium carbonate (15 g, 47 mmol) in DMF (50 mL) was added 2,2,2-trifluoroethyl trifluoromethane-sulfonate (11 mL, 47 mmol) dropwise. The reaction mixture was stirred at room temperature for 1 hour. After being stirred at room temperature for 18 hours, the mixture was poured into H2O, and the aqueous phase was extracted with ethyl acetate (twice). The combined organic layers were dried over magnesium sulfate and concentrated in vacuo to give 8.3 g (quantitative yield) of the title compound as a brown oil:
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09101616B2 |
| Quelldatensatz | uspto-grants-2015_08 |
| ORD ID | ord-772556a1c68b411b84ff083a4711911e |
| Quellennotiz | uspto-grants-2015_08 |