Reaktion #214059

ord-8ed1ffc6bae54fa19ff776cae9dfd5dc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 15 hours
  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
    Waschenthe methylene chloride mixture was washed three times with 250 ml of water each time
  8. 8
    Trocknendried over sodium sulphate
  9. 9
    workup.DISTILLATIONdistilled

Vorschrift

213.5 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 under reflux for 15 hours and 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 was taken up in 1,000 ml of methylene chloride and the methylene chloride mixture was washed three times with 250 ml of water each 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 were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04254132uspto-grants-1981_03