HRID2056966
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux for 7 hours under a nitrogen atmosphere
- temperatureto cool
- customprecipitated out
- filtrationThis material was filtered off
- washwashed with water
- dry with materialdried under vacuum over phosphorous pentoxide