HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → HCID 1714247, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | Ethyl 6-chloro-2-oxo-4-phenyl-1,2-dihydro-3-quinolinecarboxylate | HCID 738703 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 1714247 | HCID 1714247 | 63% |
Reaktionsschritte
POCl3 (15 ml) was added to 6-chloro-2-oxo-4-phenyl-1,2-dihydro-quinoline-3-carboxylic acid ethyl ester (3 g, 9.15 mmol) and refluxed for 1 h. Then the reaction mixture was cooled to room temperature and diluted with cold water and the pH was adjusted to 7 with ammonia solution and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, concentrated in vacuo to afford a crude residue which was purified by flash column chromatography (100-200 mesh silica, eluting with 5-10% ethyl acetate in hexane) to afford pure 2,6-dichloro-4-phenyl-quinoline-3-carboxylic acid ethyl ester (2 g, 63%) as pale yellow solid. LC-MS: 346 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09199938B2 |
| Quelldatensatz | uspto-grants-2015_12 |
| ORD ID | ord-90bec080609046b5b16307b105bb7b44 |
| Quellennotiz | uspto-grants-2015_12 |