Potassium Carbonate → HCID 20286598, Verbindung

HRID 127239

Reaktionsgleichung

Reaktionsgleichung von HRID 127239
Br[CH2:2][C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6].[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:6][CH2:5][C:4]([CH3:8])([CH3:7])[C:3](=[O:9])[CH2:2][O:23][C:20]1[CH:19]=[CH:18][C:17]([C:14]2[CH:15]=[CH:16][C:11]([Cl:10])=[CH:12][CH:13]=2)=[CH:22][CH:21]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 915894'-Chloro-4-biphenylolHCID 104207672-Butanone, 1-bromo-4-chloro-3,3-dimethyl-

Produkt 1

HCID 20286598HCID 20286598, VerbindungAusbeute 55,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

42.7 g (0.2 mol) of 1-bromo-4-chloro-3,3-dimethyl-butan-2-one were added dropwise to a boiling suspension of 41 g (0.2 mol) of 4-(4-chlorophenyl)-phenol and 28 g (0.2 mol) of potassium carbonate in 300 ml of absolute acetone. The mixture was stirred for 15 hours under reflux and was then allowed to cool and the inorganic residue was filtered off and rinsed with acetone. The filtrate was concentrated by distilling off the solvent in vacuo. The residue crystallized after the addition of 50 ml of diisopropyl ether. 37.5 g (55% of theory) of 4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-butan-2-one of melting point 67°-68° C. were obtained.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureto cool
  3. filtrationthe inorganic residue was filtered off
  4. washrinsed with acetone
  5. concentrationThe filtrate was concentrated
  6. distillationby distilling off the solvent in vacuo
  7. customThe residue crystallized
  8. additionafter the addition of 50 ml of diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-68c453afb2d64ef2b7b89777c2689575
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255434

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