Reaktion #214059
ord-8ed1ffc6bae54fa19ff776cae9dfd5dc
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1Temperaturunder reflux for 15 hours
- 2Temperaturto cool
- 3Filtrationthe inorganic residue was filtered off
- 4Waschenrinsed with acetone
- 5EinengenThe filtrate was concentrated
- 6workup.DISTILLATIONby distilling off the solvent in vacuo
- 7Waschenthe methylene chloride mixture was washed three times with 250 ml of water each time
- 8Trocknendried over sodium sulphate
- 9workup.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.