HRID354684

反应详情

EQUATION

反应方程式

HRID 354684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 80 ml of toluene is dissolved 5.9 g of 2,4,5-trimethoxybenzaldehyde, followed by addition of 4.8 g of diethyl malonate, 0.3 ml of piperidine and 0.3 g of benzoic acid. The mixture is heated under reflux for 4 hours, water being removed via an ester tube. After cooling, the solvent is distilled off under reduced pressure and the residual crystals are recovered by filtration with n-hexane to give 8.9 g (87.3%) of diethyl 2,4,5-trimethoxybenzylidenemalonate, m.p. 86°-87° C.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 4 hours
  3. customwater being removed via an ester tube
  4. temperatureAfter cooling
  5. distillationthe solvent is distilled off under reduced pressure
  6. filtrationthe residual crystals are recovered by filtration with n-hexane