HRID1089355

反应详情

EQUATION

反应方程式

HRID 1089355 的结构方程式

PROCEDURE

实验过程

A mixture of 67.6 g (0.02 mole) 1-(3',5'-dibromo-4'-acetoxyphenyl)ethanol, 0.35 g freshly melted and then finely pulverized potassium hydrogen sulfate, and 0.5 g t-butylhydroquinone are heated at 20 Torr to 170°-190° C. The resulting product is distilled off (under vacuum) at a temperature of 140° to 160° C. It is taken up in ether, the ether solution is washed with Na2CO3, dried, and concentrated under vacuum. The remaining product is distilled at 0.02 mbar; the boiling point is 116° C. The isolated product, which is a highly viscous oil or a white, waxy solid, has a melting point of approximately 75° C. The reaction yield is 27 g.

WORKUP

后处理

  1. distillationThe resulting product is distilled off (under vacuum) at a temperature of 140° to 160° C
  2. washthe ether solution is washed with Na2CO3
  3. customdried
  4. concentrationconcentrated under vacuum
  5. distillationThe remaining product is distilled at 0.02 mbar
  6. customThe reaction yield is 27 g