Reaktion #214418
ord-d5fa27dfe783477ba495ec12cf37b38e
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1Temperaturunder reflux
- 2Temperaturto cool
- 3Filtrationthe inorganic residue was filtered off
- 4Waschenrinsed with acetone
- 5EinengenThe filtrate was concentrated
- 6workup.DISTILLATIONby distilling off the solvent in vacuo
- 7Waschenwashed three times with 250 ml of water at a time
- 8Trocknendried over sodium sulphate
- 9workup.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.