Sulfuryl chloride → 1-([1,1′-Biphenyl]-4-yloxy)-1-chloro-3,3-dimethyl-2-butanone

HRID 972750Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 972750
[C:1]1([C:7]2[CH:20]=[CH:19][C:10]([O:11][CH2:12][C:13](=[O:18])[C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(Cl)([Cl:24])(=O)=O>C(Cl)Cl>[Cl:24][CH:12]([O:11][C:10]1[CH:9]=[CH:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:20][CH:19]=1)[C:13](=[O:18])[C:14]([CH3:16])([CH3:17])[CH3:15]

Komponenten

4

Edukt 2

HCID 24648Sulfuryl chlorideHCID 230504261-([1,1′-Biphenyl]-4-yloxy)-3,3-dimethyl-2-butanone

Produkt 1

HCID 150706801-([1,1′-Biphenyl]-4-yloxy)-1-chloro-3,3-dimethyl-2-butanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

1,292 g (4.83 moles) of 1-(4'-phenyl-phenoxy)-3,3-dimethylbutan-2-one were dissolved in 2.5 l of methylene chloride and 400 ml (4.9 moles) of sulfuryl chloride were added dropwise at the boil. The mixture was heated under reflux for 15 hours and was then concentrated by distilling off the solvent. After adding 250 ml of carbon tetrachloride, the solvent was again distilled off under a water-pump vacuum (bath temperature 65° C.). Crude 1-chloro-1-(4'-phenyl-phenoxy)-3,3-dimethylbutan-2-one was obtained quantitatively, and was used further in the form obtained. ##STR3##

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 15 hours
  3. concentrationwas then concentrated
  4. distillationby distilling off the solvent
  5. additionAfter adding 250 ml of carbon tetrachloride
  6. distillationthe solvent was again distilled off under a water-pump vacuum (bath temperature 65° C.)

Quellen und Nachweise

ORD-Eintrag
ord-b2e693431eb244a193848d0f447126be
Quelldatensatz
uspto-grants-1977_10
Patentnummer
US04053616

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