HRID2056966

反应详情

EQUATION

反应方程式

HRID 2056966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dimethyl 2,5-bis{(4-bromophenyl}amino]cyclohexa-1,4-diene-1,4-dicarboxylate (5.36 gm; 10 mmol) the sodium salt of 3-nitrobenzenesulphonic acid (2.3 gm; 10 mmol), ethanol (50 ml) and 1.0M sodium hydroxide (30 ml) were heated to reflux for 7 hours under a nitrogen atmosphere. The bright yellow solution was allowed to cool and water (120 ml) was added. The mixture was acidified with conc. hydrochloric acid when a magenta solid precipitated out. This material was filtered off, washed with water and dried under vacuum over phosphorous pentoxide to give 4.84 gm (96%) of 2,5-bis{(4-bromophenyl)amino}terephthalic acid.

WORKUP

后处理

  1. temperatureto reflux for 7 hours under a nitrogen atmosphere
  2. temperatureto cool
  3. customprecipitated out
  4. filtrationThis material was filtered off
  5. washwashed with water
  6. dry with materialdried under vacuum over phosphorous pentoxide