HRID127239

反应详情

EQUATION

反应方程式

HRID 127239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

42.7 g (0.2 mol) of 1-bromo-4-chloro-3,3-dimethyl-butan-2-one were added dropwise to a boiling suspension of 41 g (0.2 mol) of 4-(4-chlorophenyl)-phenol and 28 g (0.2 mol) of potassium carbonate in 300 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. The residue crystallized after the addition of 50 ml of diisopropyl ether. 37.5 g (55% of theory) of 4-chloro-1-[4-(4-chlorophenyl)-phenoxy]-3,3-dimethyl-butan-2-one of melting point 67°-68° C. were obtained.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureto cool
  3. filtrationthe inorganic residue was filtered off
  4. washrinsed with acetone
  5. concentrationThe filtrate was concentrated
  6. distillationby distilling off the solvent in vacuo
  7. customThe residue crystallized
  8. additionafter the addition of 50 ml of diisopropyl ether