Reaktionsgleichung
S(=O)(=O)(O)O.[F:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[F:15])[CH:10]=[O:11].[N+:16]([O-])([OH:18])=[O:17]>>[F:6][C:7]1[CH:8]=[C:9]([C:12]([N+:16]([O-:18])=[O:17])=[CH:13][C:14]=1[F:15])[CH:10]=[O:11]Komponenten
Reaktionsbedingungen
- Temperatur
- 5 °C
Versuchsvorschrift
To 520 cm3 of sulphuric acid, cooled to 0° C., are added, with stirring, 60 cm3 of fuming nitric acid, over 30 minutes. 100 g of 3,4-difluorobenzaldehyde are added over 30 minutes at approximately 0° C. to the solution obtained. The temperature is allowed to return to approximately 20° C. and stirring is continued for 3 hours at this temperature. After cooling to approximately 5° C., the reaction mixture is poured, over 30 minutes and with vigorous stirring, onto 1200 g of crushed ice. The temperature is allowed to return to approximately 20° C., followed by extraction with twice 600 cm3 of toluene. The combined organic extracts are washed with 3 times 1000 cm3 of water, and concentrated under reduced pressure (20 kPa) at 50° C. 113 g of 3,4-difluoro-6-nitrobenzaldehyde are obtained in the form of a brown oil, which is used as it is in the subsequent syntheses. A purified sample of 3,4-difluoro-6-nitrobenzaldehyde gives the following characteristics:
Aufarbeitung
- additionare added
- customobtained
- customto return to approximately 20° C.
- stirringstirring
- customto return to approximately 20° C.
- extractionfollowed by extraction with twice 600 cm3 of toluene
- washThe combined organic extracts are washed with 3 times 1000 cm3 of water
- concentrationconcentrated under reduced pressure (20 kPa) at 50° C
Quellen und Nachweise
- ORD-Eintrag
- ord-eddde3e0a98249119dc51c1baddd3cbe
- Quelldatensatz
- uspto-grants-1997_04
- Patentnummer
- US05624933
Verknüpfte Notizen
Wird geladen…