HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → 1-(3,5-Dichloro-2-pyridyl)-3-trifluoromethylpropane-1,3-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | 2,2,2-Trifluoroethyl Acetate | HCID 136256 | — |
| Edukt | Sodium ethoxide | HCID 2723922 | — |
| Edukt | 1-(3,5-Dichloropyridin-2-yl)ethanone | HCID 21712163 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1-(3,5-Dichloro-2-pyridyl)-3-trifluoromethylpropane-1,3-dione | HCID 21712152 | — |
Reaktionsschritte
15.8 g of 3,5-dichloro-2-acetylpyridine are introduced together with 12.0 ml of trifluoroethyl acetate into 125 ml of absolute ether. With stirring, the mixture is cooled using an ice-bath and 46.6 ml of, a 21% sodium ethanolate solution in ethanol are added dropwise. The ice-bath is then removed and the mixture is subsequently stirred overnight at 25° C. After cooling the reaction mixture in an ice-bath and adding dropwise 7.5 ml of glacial acetic acid, the mixture is concentrated in vacuo. 39.0 g of 1-(3,5-dichloro-2-pyridyl)-3-trifluoromethylpropane-1,3-dione are obtained, which can be used directly for the following cyclisation step.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06274536B1 |
| Quelldatensatz | uspto-grants-2001_08 |
| ORD ID | ord-d48b8b86d8ba4b78b29c8927f41d80b5 |
| Quellennotiz | uspto-grants-2001_08 |