HRID133687

反应详情

EQUATION

反应方程式

HRID 133687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

36.3 g (0.3 mol) of p-aminobenzaldehyde are suspended in 450 ml of isopropanol. A mixture of 59.1 g (0.3 mol) of 2-ethylhexyl cyanoacetate and of catalyst (0.375 ml of diethylamine and 1.125 ml of acetic acid) is introduced therein. The mixture is refluxed for 5 hours. The same amount of catalyst is added again and refluxing is continued for a further 4 hours. The insoluble materials are removed by hot filtration and the mixture is concentrated to a volume of 300 ml and left to crystalize. After filtration and drying, 59.6 g (66% yield) of an orange-coloured powder are obtained, and are used without further purification for the following step.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 5 hours
  2. additionThe same amount of catalyst is added again
  3. temperaturerefluxing
  4. customThe insoluble materials are removed by hot filtration
  5. concentrationthe mixture is concentrated to a volume of 300 ml
  6. waitleft
  7. customto crystalize
  8. filtrationAfter filtration
  9. customdrying