Potassium Carbonate → 2-Fluoro-6-nitrobenzoic acid

HRID 67597

Reaktionsgleichung

Reaktionsgleichung von HRID 67597
[F:1][C:2]1[C:7](C)=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:4][CH:3]=1.[C:12](=[O:15])([O-])[O-:13].[K+].[K+].[Mn]([O-])(=O)(=O)=O.[K+].[Mn]([O-])(=O)(=O)=O>O>[F:1][C:2]1[C:7]([C:12]([OH:13])=[O:15])=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 24401PermanganateHCID 698542-Fluoro-6-nitrotolueneHCID 516875Potassium Permanganate

Produkt 1

HCID 6037582-Fluoro-6-nitrobenzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 34.5 g (0.22 mol) of 6-fluoro-2-nitrotoluene, 30.7 g (0.22 mol) of potassium carbonate, 105.4 g (0.66 mol) of potassium permanganate and 3.3 liters of water is heated at 100° C. until the permanganate is decolorised (ca 2.5 hours). After cooling and removal of the unreacted 6-fluoro-2-nitrotoluene by extraction with ethyl acetate, the aqueous phase is adjusted to pH 1 with hydrochloric acid and extracted three times with ethyl acetate. The combined organic extracts are dried over magnesium sulphate and concentrated, there being obtained 6-fluoro-2-nitrobenzoic acid. After recrystallisation from ethyl acetate/n-hexane, the product melts at 146°-148° C.

Aufarbeitung

  1. custom(ca 2.5 hours)
  2. temperatureAfter cooling
  3. customremoval of the unreacted 6-fluoro-2-nitrotoluene
  4. extractionby extraction with ethyl acetate
  5. extractionextracted three times with ethyl acetate
  6. dry with materialThe combined organic extracts are dried over magnesium sulphate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-fba7179408844ffb8b676519c0e18e98
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346036

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