Реакция #349632

Уравнение реакции

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

4-chlorophenol

potassium carbonate

→

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

Выход 74.6%

Растворители

acetone

acetone

Условия реакции

Обработка

1. 1
   ТемператураAfter heating for 15 hours
2. 2
   Температураunder reflux
3. 3
   Фильтрацияthe mixture was filtered
4. 4
   Концентрированиеthe filtrate was concentrated
5. 5
   workup.DISTILLATIONby distilling off the solvent in vacuo
6. 6
   Промывкаthe solution was washed three times with 50 ml of water at a time
7. 7
   Сушкаdried over sodium sulphate
8. 8
   Концентрированиеconcentrated
9. 9
   workup.DISTILLATIONThe oily residue was distilled

Методика

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.

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