Sodium Iodide → HCID 21995698, Verbindung

HRID 1978737Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1978737
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([CH3:9])[C:3]=1[CH3:10].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:20][CH2:21][O:22][CH2:23][CH2:24][CH3:25]>CN(C=O)C.O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:20][CH2:21][O:22][CH2:23][CH2:24][CH3:25])=[C:4]([CH3:9])[C:3]=1[CH3:10]

Komponenten

7

Edukt 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 1235061-(2-Chloroethoxy)propaneHCID 139746564-Bromo-2,3-dimethylphenol

Produkt 1

HCID 21995698HCID 21995698, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

In DMF (82 ml) was dissolved 4-bromo-2,3-dimethylphenol (8.2 g). To the mixture were added potassium carbonate (7.3 g) and sodium iodide (6.1 g) and then was added dropwise 2-chloroethylpropylether (6.2 ml), and the mixture was stirred at 90 for 10 hours and cooled to room temperature. The reaction mixture was added to water, and the mixture was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (hexane/ethyl acetate=12/1) to give 4-bromo-2,3-dimethyl-1-(2-propoxyethoxy)benzene (7.5 g).

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried with magnesium sulfate
  4. customUnder reduced pressure, the solvent was evaporated
  5. customthe residue was purified with silica gel column chromatography (hexane/ethyl acetate=12/1)

Quellen und Nachweise

ORD-Eintrag
ord-01afa9d67e644610905bb7bfc7e5f6a4
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06235771B1

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