HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → Ethyl 2-[2,5-difluorobenzoyl]-3-dimethylamino-2-propenoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Ethyl 3-(N,N-dimethylamino)acrylate | HCID 121015 | — |
| Edukt | 2,5-Difluorobenzoyl chloride | HCID 588082 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | Ethyl 2-[2,5-difluorobenzoyl]-3-dimethylamino-2-propenoate | HCID 68584816 | 11,3% |
Reaktionsbedingungen
| Temperatur | 90 °C |
|---|
Reaktionsschritte
A solution of 2,5-difluorobenzoyl chloride (5.26 g, 29.8 mmol) in toluene (100 mL) was treated with ethyl-3-(dimethylamino)-2-propenoate (5.27 g, 36.8 mmol), followed by triethylamine (5.9 mL, 42.5 mmol). The mixture was stirred at 90° C. for 6.5 h then allowed to cool, and the precipitate removed by filtration. The filtrate was concentrated under reduced pressure to give a residue which was purified by flash chromatography (silica gel, 50-100% diethyl ether in petroleum ether [b.p. 40-60° C.]) to give the title compound as a yellow oil (0.95 g); ESMS m/z 284.4 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07718621B2 |
| Quelldatensatz | uspto-grants-2010_05 |
| ORD ID | ord-e889998953af434a9fd929934d35e758 |
| Quellennotiz | uspto-grants-2010_05 |