HRID256276

反应详情

EQUATION

反应方程式

HRID 256276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a round bottom flask equipped with stirrer, thermometer, and nitrogen inlet is added 2.77 g (0.1M) 1,5-bischloroanthraquinone and 3.5 g (0.2M) of 4-cyclohexylaniline. 3.0 g anhydrous sodium acetate and 0.1 g anhydrous copper acetate are added as acid acceptor and reaction catalyst respectively. 50 g nitrobenzene are added and the stirred mass is heated to reflux under nitrogen atmosphere. The reaction is allowed to proceed for two hours at 185° C. Upon cooling, 50 g methanol is added and the crude dye separated by vacuum filtration. Subsequent purification by recrystalization and chromatography from alumina using toluene as the elvent affords the magneta pleochroic dye 1,5-bis(4-cyclohexylphenylamino)-anthraquinone. The optical order parameter was measured as 0.7.

WORKUP

后处理

  1. customIn a round bottom flask equipped with stirrer
  2. customacceptor and reaction catalyst respectively
  3. temperaturethe stirred mass is heated
  4. temperatureto reflux under nitrogen atmosphere
  5. temperatureUpon cooling
  6. customthe crude dye separated by vacuum filtration
  7. customSubsequent purification
  8. customby recrystalization and chromatography from alumina