Ethyl Acetate → HCID 23042157, Verbindung

HRID 2166101Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2166101
[O:1]([C:8]1[CH:13]=[CH:12][C:11](O)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15](=[O:18])([O-])[O-].[K+].[K+].[Br:21][C:22]1[S:23][CH:24]=[C:25](CCl)[CH:26]=1.C(OCC)(=O)C>CN(C)C=O>[Br:21][C:22]1[S:23][CH:24]=[C:25]([CH2:15][O:18][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[O:1][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:26]=1

Komponenten

6

Edukt 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 132544-PhenoxyphenolHCID 128741092-Bromo-4-(chloromethyl)thiophene

Produkt 1

HCID 23042157HCID 23042157, VerbindungAusbeute 113,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

7.44 g of 4-phenoxyphenol and 5.52 g of potassium carbonate are stirred in 50 ml of anhydrous dimethylformamide for 1 hour at 70° C. 5.52 g of 2-bromo-4-chloromethylthiophene is then dripped in, and the mixture is stirred for a further 12 hours at 80° C., and at room temperature (approx. 20° C.) overnight. The mixture is then stirred into 500 ml of ethyl acetate and washed three times with water. After drying over sodium sulfate and removal of the solvent, the residue is recrystallized from n-hexane. There is obtained 10.7 g of 2-bromo-4-[(phenoxyphenoxy)-methyl]-thiophene; colorless powder; m.p.: 90° C.

Aufarbeitung

  1. customat room temperature
  2. custom(approx. 20° C.) overnight
  3. washwashed three times with water
  4. dry with materialAfter drying over sodium sulfate and removal of the solvent
  5. customthe residue is recrystallized from n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-ec1b8f9b6ccb498997b34037395a1d9a
Quelldatensatz
uspto-grants-1990_07
Patentnummer
US04943584

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