HRID399179

反应详情

EQUATION

反应方程式

HRID 399179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

8.9 Parts of 2,5-di(p-chloroanilino)-3,6-dihydroterephthalic acid dimethyl ester, 50 parts of ethanol, 5.37 parts of KOH, 24.35 parts of water and 6 parts of sodium m-nitrobenzenesulfonate were charged into a 200-ml flask of stainless steel, and refluxed with stirring for 10 hours. When the suspension changed to a black solution, ethanol was steam-distilled, and the reaction mixture was filtered to remove a solid. The remaining solution was heated up to 80° C. with stirring, and after 35 parts of a 10% hydrochloric acid aqueous solution was dropwise added, the mixture was maintained for 1 hour. Then, the mixture was filtered, washed with hot water and dried to give 8.21 parts (98.4% of the theoretical yield) of 2,5-di(p-chloroanilino)terephthalic acid.

WORKUP

后处理

  1. temperaturerefluxed
  2. distillationwas steam-distilled
  3. filtrationthe reaction mixture was filtered
  4. customto remove a solid
  5. stirringwith stirring
  6. additionafter 35 parts of a 10% hydrochloric acid aqueous solution was dropwise added
  7. temperaturethe mixture was maintained for 1 hour
  8. filtrationThen, the mixture was filtered
  9. washwashed with hot water
  10. customdried
  11. customto give 8.21 parts (98.4% of the