Iodine → 2-Iodo-4,5-dimethylphenol

HRID 228686

Reaktionsgleichung

Reaktionsgleichung von HRID 228686
[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[CH3:8].[I:10]I.S([O-])([O-])=O.[Na+].[Na+]>CO.O>[I:10][C:5]1[CH:6]=[C:7]([CH3:8])[C:2]([CH3:1])=[CH:3][C:4]=1[OH:9]

Komponenten

5

Edukt 3

HCID 807IodineHCID 72493,4-DimethylphenolHCID 24437Sodium Sulfite

Produkt 1

HCID 136352572-Iodo-4,5-dimethylphenolAusbeute 64 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 22242641Methanol--water (1/1)Lösungsmittel

Versuchsvorschrift

3,4-Dimethylphenol (0.68 g) and iodine (1.82 g) were dissolved in methanol/water (10 ml/5 ml), and the mixture was stirred at room temperature overnight. An aqueous sodium sulfite solution was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography using ethyl acetate-hexane to give 2-iodo-4,5-dimethylphenol (833 mg, yield 64%).

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was then washed with water
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customThe residue was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-3986cdf6743c42169ba8bf3e20a19168
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07560558B2

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