HRID616652

反应详情

EQUATION

反应方程式

HRID 616652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a diethyl ether solution of ethylidenetriphenylphosphorane prepared in the usual way from 800 g. of ethyltriphenylphosphonium bromide, 400 g. of ethyl 3,4-dimethoxyphenylglyoxylate in 600 ml. of ether are added dropwise. After refluxing for 4-5 hours, the solvent is evaporated and substituted with tetrahydrofuran. The mixture is then heated for 36 hours and then evaporated to dryness and the residue is extracted with diethyl ether in a Soxhlet apparatus giving 150 g. of the title compound. Pursuant to this procedure, the following other α-arylcrotonate starting materials are prepared:

WORKUP

后处理

  1. temperatureAfter refluxing for 4-5 hours
  2. customthe solvent is evaporated
  3. temperatureThe mixture is then heated for 36 hours
  4. customevaporated to dryness
  5. extractionthe residue is extracted with diethyl ether in a Soxhlet apparatus
  6. customgiving 150 g