1-Chloro-2,4,6-trifluorobenzene → 1,3,5-Trifluorobenzene

HRID 1721515

Reaktionsgleichung

Reaktionsgleichung von HRID 1721515
Cl[C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[CH:4][C:3]=1[F:10]>[Cu].[Zn].S([O-])([O-])(=O)=O.[Cu+2].[Zn].O>[F:8][C:7]1[CH:2]=[C:3]([F:10])[CH:4]=[C:5]([F:9])[CH:6]=1

Komponenten

6

Edukt 1

HCID 27366621-Chloro-2,4,6-trifluorobenzene

Produkt 1

HCID 97451,3,5-TrifluorobenzeneAusbeute 42 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 23994ZincKatalysatorHCID 24462Copper SulfateKatalysatorHCID 10290809Zinc copper coupleKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
330 °C

Versuchsvorschrift

An autoclave was charged with 6.68 g of 2-chloro-1,3,5-trifluorobenzene, 0.5 g of water and 7.5 g of 3-5% zinc-copper couple (prepared by adding an aqueous solution of copper sulfate to an aqueous dispersion of zinc powder (copper/zinc weight ratio of 3 to 5%), allowing the mixture to stand, filtering out the solid component under reduced pressure, and washing, drying and pulverizing the solid component in a mortar), and the content was heated at 330° C. with high speed stirring for 32 hours. After the reaction, the content was distilled off, and a fraction distilled off at 74° to 77° C. was dried over sodium sulfate to obtain 1,3,5-trifluorobenzene in an amount of 2.19 g (yield 42%).

Aufarbeitung

  1. customprepared
  2. filtrationfiltering out the solid component under reduced pressure
  3. washwashing
  4. customdrying
  5. customAfter the reaction
  6. distillationthe content was distilled off
  7. distillationa fraction distilled off at 74° to 77° C.
  8. dry with materialwas dried over sodium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-7ab27560425f41dbbe58ca1101c9c981
Quelldatensatz
uspto-grants-1996_04
Patentnummer
US05510533

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