Potassium Nitrate → Benzoic acid,2,3,6-trifluoro-5-nitro-

HRID 1638663

Reaktionsgleichung

Reaktionsgleichung von HRID 1638663
[F:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]([F:12])[C:3]=1[C:4]([OH:6])=[O:5].[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[F:12][C:7]1[C:8]([N+:13]([O-:15])=[O:14])=[CH:9][C:10]([F:11])=[C:2]([F:1])[C:3]=1[C:4]([OH:6])=[O:5]

Komponenten

4

Edukt 2

HCID 24434Potassium NitrateHCID 5200622,3,6-Trifluorobenzoic acid

Produkt 1

HCID 15631828Benzoic acid,2,3,6-trifluoro-5-nitro-Ausbeute 83,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel2×

Versuchsvorschrift

2,3,6-Trifluorobenzoic acid (21.0 g) is added to conc. sulfuric acid (120 ml) under ice-cooling. To the mixture is added dropwise a solution of potassium nitrate (14.5 g) in conc sulfuric acid (30 ml) at below 20° C. After the addition, the mixture is stirred at room temperature for one hour. The reaction mixture is poured into ice water and extracted with diethyl ether. The extract is dried over magnesium sulfate, and then the solvent is distilled off. The residue is recrystallized from dichloromethane-n-hexane to give 2,5,6-trifluoro-3-nitrobenzoic acid (22 g), as colorless prisms, m.p. 98°-99° C.

Aufarbeitung

  1. temperaturecooling
  2. additionAfter the addition
  3. extractionextracted with diethyl ether
  4. dry with materialThe extract is dried over magnesium sulfate
  5. distillationthe solvent is distilled off
  6. customThe residue is recrystallized from dichloromethane-n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-b5254972de5341e0b25ff1d9a8773f6d
Quelldatensatz
uspto-grants-1989_11
Patentnummer
US04880806

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