Reaktion #214418

ord-d5fa27dfe783477ba495ec12cf37b38e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux
  2. 2
    Temperaturto cool
  3. 3
    Filtrationthe inorganic residue was filtered off
  4. 4
    Waschenrinsed with acetone
  5. 5
    EinengenThe filtrate was concentrated
  6. 6
    workup.DISTILLATIONby distilling off the solvent in vacuo
  7. 7
    Waschenwashed three times with 250 ml of water at a time
  8. 8
    Trocknendried over sodium sulphate
  9. 9
    workup.DISTILLATIONdistilled

Vorschrift

213 g (1 mol) of 1-bromo-4-chloro-3,3-dimethyl-butan-2-one were added dropwise to a boiling suspension of 128.5 g (1 mol) of 4-chlorophenol and 140 g (1 mol) of potassium carbonate in 1,000 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 and the residue was taken up in 1,000 ml of methylene chloride, washed three times with 250 ml of water at a time, dried over sodium sulphate and distilled. 210 g (80.7% of theory) of 4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one of boiling point 125°-127° C./0.1 mm Hg were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04255434uspto-grants-1981_03