HRID1729123

反应详情

EQUATION

反应方程式

HRID 1729123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 400 parts of terephthaldehyde, 120 parts of acetic acid and 300 parts of acetic anhydride was refluxed for two hours. 188 parts of 4-picoline were then added over a period of 45 minutes, and the dark brown mixture was refluxed for a further 2 hours. 3300 parts of 1M aqueous hydrochloric acid were then added. The desired product was extracted with toluene and treated with 5M sodium hydroxide to a pH between 5 and 6. The crude solid product was dissolved in hot ethyl acetate and the solution was filtered. Cooling of the filtrate gave the desired product, 4-(2-(4-formylphenyl)-ethenyl)-pyridine.

WORKUP

后处理

  1. temperaturewas refluxed for two hours
  2. temperaturethe dark brown mixture was refluxed for a further 2 hours
  3. extractionThe desired product was extracted with toluene
  4. additiontreated with 5M sodium hydroxide to a pH between 5 and 6
  5. dissolutionThe crude solid product was dissolved in hot ethyl acetate
  6. filtrationthe solution was filtered
  7. temperatureCooling of the filtrate