Nitric Acid → 6-Fluoro-3-nitro-2-trifluoromethyl-benzoic acid

HRID 2293610

Reaktionsgleichung

Reaktionsgleichung von HRID 2293610
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[F:10][C:11]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[C:12]=1[C:13]([OH:15])=[O:14].O>ClCCl>[F:10][C:11]1[C:12]([C:13]([OH:15])=[O:14])=[C:16]([C:20]([F:21])([F:22])[F:23])[C:17]([N+:1]([O-:4])=[O:2])=[CH:18][CH:19]=1

Komponenten

6

Edukt 4

HCID 944Nitric AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 6881232-Fluoro-6-(trifluoromethyl)benzoic acid

Produkt 1

HCID 214773526-Fluoro-3-nitro-2-trifluoromethyl-benzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

1.05 ml (23.3 mmol) of concentrated nitric acid (65%), which also was precooled to 0° C., is instilled in a solution of 17.5 ml of concentrated sulfuric acid and 2.5 g (12.0 mmol) of 2-fluoro-6-trifluoromethyl-benzoic acid, cooled to 0° C. It is allowed to stir for one more hour at 0° C. and then overnight at room temperature. It is then poured in a mixture of ice, water and dichloromethane, the organic phase is separated and the aqueous phase is extracted with dichloromethane. The organic solutions are combined, washed with saturated sodium chloride solution, dried on sodium sulfate and evaporated to dryness in a vacuum. The title compound is obtained in crystalline form.

Aufarbeitung

  1. customalso was precooled to 0° C.
  2. customovernight
  3. customat room temperature
  4. customthe organic phase is separated
  5. extractionthe aqueous phase is extracted with dichloromethane
  6. washwashed with saturated sodium chloride solution
  7. customdried on sodium sulfate
  8. customevaporated to dryness in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-62788c37a7ea49d1ad1694bc8f5df3e4
Quelldatensatz
uspto-grants-1997_11
Patentnummer
US05686492

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