HRID596520

反应详情

EQUATION

反应方程式

HRID 596520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

96 g of β-ionone are dissolved in 500 ml of isopropenyl acetate and treated with 0.6 g of p-toluenesulphonic acid monohydrate. The mixture is stirred at reflux temperature under an inert gas atmosphere for 24 hours. The excess isopropenyl acetate is distilled off from the mixture under a vacuum (temperature ≤50° ) and then the mixture is treated several times with hexane in order to liberate residual amounts of isopropenyl acetate and concentrated again. In this manner, there are obtained 108 g of brown-red 4-(2,6,6-trimethyl-2-cyclohexen-1-ylidene)-2-acetoxy-but-2-ene (formula II; R = acetyl).

WORKUP

后处理

  1. temperatureat reflux temperature under an inert gas atmosphere for 24 hours
  2. distillationThe excess isopropenyl acetate is distilled off from the mixture under a vacuum (temperature ≤50° )
  3. additionthe mixture is treated several times with hexane in order
  4. concentrationconcentrated again