Reaktion #349632

Reaktionsgleichung

4-acetoxy-1-bromo-3,3-dimethylbutan-2-one

4-chlorophenol

potassium carbonate

→

4-acetoxy-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one

Ausbeute 74.6%

Lösungsmittel

acetone

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter heating for 15 hours
2. 2
   Temperaturunder reflux
3. 3
   Filtrationthe mixture was filtered
4. 4
   Einengenthe filtrate was concentrated
5. 5
   workup.DISTILLATIONby distilling off the solvent in vacuo
6. 6
   Waschenthe solution was washed three times with 50 ml of water at a time
7. 7
   Trocknendried over sodium sulphate
8. 8
   Einengenconcentrated
9. 9
   workup.DISTILLATIONThe oily residue was distilled

Vorschrift

170 g (0.72 mol) of 4-acetoxy-1-bromo-3,3-dimethylbutan-2-one in 200 ml of acetone were added dropwise, over the course of 100 minutes, to a suspension of 92.1 g (0.72 mol) of 4-chlorophenol and 108 g (0.72 mol) of potassium carbonate in 1,000 ml of acetone. After heating for 15 hours whilst stirring under reflux, the mixture was filtered and the filtrate was concentrated by distilling off the solvent in vacuo. The residue was taken up in 200 ml of methylene chloride and the solution was washed three times with 50 ml of water at a time, dried over sodium sulphate and concentrated. The oily residue was distilled. 153 g (72% of theory) of 4-acetoxy-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one of boiling point 140°-145° C./0.2 mm Hg was obtained.

Quelle