Dimethyl Sulfate → Flosequinan

HRID 1155520Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1155520
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:15])[CH:7]([S:12]([CH3:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1.[C:16](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(=O)CC>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:15])[C:7]([S:12]([CH3:14])=[O:13])=[CH:8][N:9]2[CH3:16])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 705794307-Fluoro-3-methylsulphinyl-4-quinolone

Produkt 1

HCID 4474062Flosequinan

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

7-Fluoro-3-methylsulphinyl-4-quinolone (5.0 g.) was dissolved in hot butanone (250 ml.) containing anhydrous potassium carbonate (3.06 g.). The resulting suspension was stirred and treated dropwise with dimethyl sulphate (2.09 ml.). The mixture was stirred and boiled under reflux for 1 hour and filtered while hot. The filtrate was allowed to cool, giving a crystalline product. The product was collected and dried to give 7-fluoro-1-methyl-3-methylsulphinyl-4-quinolone, m.p. 226°-8°.

Aufarbeitung

  1. stirringThe mixture was stirred
  2. temperatureunder reflux for 1 hour
  3. filtrationfiltered while hot
  4. temperatureto cool
  5. customgiving a crystalline product
  6. customThe product was collected
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-47a90ed0e75b4d17b3f3b5b5c34ac574
Quelldatensatz
uspto-grants-1981_11
Patentnummer
US04302460

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