Potassium Nitrate → 4-Methyl-3-nitrobenzotrifluoride

HRID 412079

Reaktionsgleichung

Reaktionsgleichung von HRID 412079
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][CH:3]=1.[N+:12]([O-])([O-:14])=[O:13].[K+].CCCCCC.C(OCC)(=O)C>S(=O)(=O)(O)O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([F:9])([F:10])[F:11])=[CH:6][C:7]=1[N+:12]([O-:14])=[O:13]

Komponenten

5

Edukt 3

HCID 24434Potassium NitrateHCID 802304-MethylbenzotrifluorideHCID 21226206Ethyl acetate hexane

Produkt 1

HCID 14728854-Methyl-3-nitrobenzotrifluorideAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel2×

Versuchsvorschrift

To a solution of 4-methylbenzotrifluoride (18.6 g, 116 mmol) in concentrated sulfuric acid (120 ml) was added dropwise a solution of potassium nitrate (12.9 g, 128 mmol) in concentrated sulfuric acid (60 ml) at room temperature over 15 minutes. After stirring for 2 hours at the same temperature, the reaction mixture was poured into ice water, which was extracted with ethyl acetate, dried over anhydrous sodium sulfate, and solvent was distilled off. The residue obtained was submitted to silica gel column chromatography [hexane-ethyl acetate=8:1] to obtain 22.8 g of title compound as pale yellow liquid. Yield 96%.

Aufarbeitung

  1. extractionwas extracted with ethyl acetate
  2. dry with materialdried over anhydrous sodium sulfate, and solvent
  3. distillationwas distilled off
  4. customThe residue obtained

Quellen und Nachweise

ORD-Eintrag
ord-53da0b72a505422f8da21304dfcbc003
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06562839B1

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