HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,6-Dimethylmorpholine → 6-Chloro-1-cyclopropyl-7-(2,6-dimethylmorpholin-4-yl)-8-fluoro-4-oxo-quinoline-3-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,6-Dimethylmorpholine | HCID 110862 | — |
| Edukt | Diazabicyclo(2.2.2)octane | HCID 136165 | — |
| Edukt | 6-Chloro-1-cyclopropyl-7,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid | HCID 13579163 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | 6-Chloro-1-cyclopropyl-7-(2,6-dimethylmorpholin-4-yl)-8-fluoro-4-oxo-quinoline-3-carboxylic acid | HCID 483106 | 41% |
Reaktionsschritte
3 g (10 mmol) of the product from Example A in 35 ml of dimethyl sulphoxide are heated at 140° with 1.2 g (10 mmol) of 2,6-dimethylmorpholine and 2.2 g (20 mmol) of diazabicyclo[2.2.2]octane for 5 hours. The mixture is concentrated under high vacuum, stirred with 30 ml of water, the pH is adjusted to 6 with 2N hydrochloric acid, and the precipitate is filtered off with suction and recrystallized from glycol monomethyl ether. 1.6 g (41% of theory) of 6-chloro-1-cyclopropyl-8-fluoro-1,4-dihydro-7-(2,6-dimethyl-4-morpholinyl)-4-oxo-3-quinolinecarboxylic acid of melting point 258°-261° (with decomposition) is obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05468861 |
| Quelldatensatz | uspto-grants-1995_11 |
| ORD ID | ord-422f5174584a4930ae1d2a19049950f0 |
| Quellennotiz | uspto-grants-1995_11 |