Sodium percarbonate → 3,4-Difluorobenzoic acid

HRID 374618

Reaktionsgleichung

Reaktionsgleichung von HRID 374618
[C:1]([O-:4])([O-])=[O:2].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[F:19][C:20]1[CH:21]=[C:22]([CH:31]=[CH:32][C:33]=1[F:34])C(C1C=CC=CC=1)=O>FC(F)(F)C(O)=O>[F:19][C:20]1[CH:21]=[C:22]([CH:31]=[CH:32][C:33]=1[F:34])[C:1]([OH:4])=[O:2]

Komponenten

4

Edukt 2

HCID 159762Sodium percarbonateHCID 5699083,4-Difluorobenzophenone

Produkt 1

HCID 991663,4-Difluorobenzoic acidAusbeute 95,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

2.5 g of sodium percarbonate were added over 1 h to a solution of 2.2 g (10 mmol) of 3,4-difluorobenzophenone and 20 ml of trifluoroacetic acid (0° C.) and the temperature was then allowed to rise to 20° C. The mixture was stirred for 16 h at this temperature and 50 g of ice were then added. The mixture was subsequently extracted twice with dichloromethane and the organic phases were washed (NaHCO3) until the washings were neutral. The solvent was then removed. Working-up as described in Example 22 gave 1.2 g (7.6 mmol, 76%) of 3,4-difluorobenzoic acid, which can be obtained analytically pure from water (melting point 113°-120.5° C.).

Aufarbeitung

  1. customto rise to 20° C
  2. additionwere then added
  3. extractionThe mixture was subsequently extracted twice with dichloromethane
  4. washthe organic phases were washed (NaHCO3) until the washings
  5. customThe solvent was then removed

Quellen und Nachweise

ORD-Eintrag
ord-3a540bda32044b3891e823049d0d41e1
Quelldatensatz
uspto-grants-1996_01
Patentnummer
US05481032

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