HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl trifluoroacetate → 4,4,4-Trifluoro-1-(pyridin-2-yl)butane-1,3-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl trifluoroacetate | HCID 9794 | — |
| Edukt | 2-Acetylpyridine | HCID 14286 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 4,4,4-Trifluoro-1-(pyridin-2-yl)butane-1,3-dione | HCID 2771478 | 81,2% |
Reaktionsschritte
Trifluoro-acetic acid ethyl ester (9.82 mL, 82.5 mmol) was added to a solution of 1-pyridin-2-yl-ethanone (5.00 g, 41.2 mmol) in methanol (40 mL) containing sodium methoxide (61.8 mmol). The reaction mixture was heated at reflux overnight, concentrated under reduced pressure and acidified with aqueous hydrochloric acid (10%). The aqueous solution was extracted with ethyl acetate (10×50 mL). The organic layers were collected, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel to give 4,4,4-trifluoro-1-pyridin-2-yl-butane-1,3-dione (7.26 g, 81%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07098335B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-041f2cc851b84257b82bcd81cc91efb6 |
| Quellennotiz | uspto-grants-2006_08 |