Reaktionsgleichung
[I-].[K+].[C:3]([CH:5]1[CH2:14][N:13]([CH3:15])[C:12]2[N:11]=[C:10]3[CH:16]=[C:17]([F:21])[C:18]([F:20])=[CH:19][C:9]3=[CH:8][C:7]=2[C:6]1=[O:22])#[N:4].OO.S([O-])([O-])(=O)=S.[Na+].[Na+]>O.C(O)C>[C:3]([C:5]1[C:6](=[O:22])[C:7]2[CH:8]=[C:9]3[CH:19]=[C:18]([F:20])[C:17]([F:21])=[CH:16][C:10]3=[N:11][C:12]=2[N:13]([CH3:15])[CH:14]=1)#[N:4]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 77 °C
Versuchsvorschrift
A solution of 0.47 g of potassium iodide in 5 cm3 of water is added with stirring at approximately 20° C. to a suspension of 8.6 g of 3-cyano-7,8-difluoro-1-methyl-4-oxo-1,2,3,4-tetrahydrobenzo[b][1,8]naphthyridine in 350 cm3 of ethanol. The suspension is heated to 77° C., and 4 cm3 of 33% by weight hydrogen peroxide are added in the course of 10 minutes at this temperature. The reaction mixture is kept refluxing for a further 30 minutes and is then cooled to approximately 20° C. 10 cm3 of 1N sodium thiosulphate solution are added in the course of 5 minutes at this temperature. The precipitate obtained is drained at approximately 20° C. and washed with twice 20 cm3 of water. The wet product obtained is dried under reduced pressure (20 kPa) at approximately 50° C. 8 g of 3-cyano-7,8-difluoro-1-methyl-4-oxo-1,4-dihydrobenzo[b]-[1,8]naphthyridine are obtained in the form of a light yellow solid, melting point 380° C.
Aufarbeitung
- temperatureThe reaction mixture is kept refluxing for a further 30 minutes
- temperatureis then cooled to approximately 20° C
- customThe precipitate obtained
- customis drained at approximately 20° C.
- washwashed with twice 20 cm3 of water
- customThe wet product obtained
- customis dried under reduced pressure (20 kPa) at approximately 50° C
Quellen und Nachweise
- ORD-Eintrag
- ord-95976bcdad274af785847ff74d74e032
- Quelldatensatz
- uspto-grants-1995_08
- Patentnummer
- US05442070
Verknüpfte Notizen
Wird geladen…