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Methyl 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoate → 4-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid

HRID 1608899
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1608899
[CH2:1]([O:5][CH2:6][C:7]([F:27])([F:26])[C:8]([F:25])([F:24])[C:9]([F:23])([F:22])[CH2:10][O:11][C:12]1[CH:21]=[CH:20][C:15]([C:16]([O:18]C)=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4]>[OH-].[K+]>[CH2:1]([O:5][CH2:6][C:7]([F:26])([F:27])[C:8]([F:24])([F:25])[C:9]([F:22])([F:23])[CH2:10][O:11][C:12]1[CH:21]=[CH:20][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4]
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Komponenten

3

Edukt 1

HCID 20082759Methyl 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoate

Produkt 1

HCID 200827564-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14797Potassium HydroxideLösungsmittel

Versuchsvorschrift

Subsequently, the methyl 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoate was heated at reflux with 20 ml of 10% aqueous KOH for 2 hours. The resulting hydrolyzed carboxylate salt reaction product mixture was then cooled to room temperature and was acidified with concentrated (98%) sulfuric acid. The desired fluorinated benzoic acid precipitate was filtered from the aqueous solution and was washed twice with 10 ml aliquots of deionized water. The product was dried in a vacuum oven at 60° C. and a pressure of 0.2 mm Hg (0.2 torr). A total of 9.5 g of the desired 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid was recovered.

Aufarbeitung

  1. concentrationwith concentrated (98%) sulfuric acid
  2. filtrationThe desired fluorinated benzoic acid precipitate was filtered from the aqueous solution
  3. washwas washed twice with 10 ml aliquots of deionized water
  4. customThe product was dried in a vacuum oven at 60° C.
  5. customA total of 9.5 g of the desired 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid was recovered

Quellen und Nachweise

ORD-Eintrag
ord-7567f8a0c6b8440395cd69dcb5947865
Quelldatensatz
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05399291

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