HRID1075130

反应详情

EQUATION

反应方程式

HRID 1075130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1-Chloro-4-hydroxyanthraquinone (27.8 gm) is dissolved in 200 ml nitrobenzene in a boiling flask fitted with a stirrer and reflux condensor. After heating to 80° C., 18.1 gm (+)-4-methylhexyl)aniline, prepared according to Example 17, is added followed by the addition of 0.1 gm copper acetate and 20 gm sodium acetate. The mixture is stirred and heated to 150° C. for 4 hours. The mixture is then cooled to 80° C. and 500 ml ethanol is added. When cooled to room temperature the crude dye is separated by filtration, water and alcohol washed, and dried overnight. Chromatography on alumina using toluene as eluent affords the pure helichromic compound. The structure of the compound is confirmed by NMR.

WORKUP

后处理

  1. customfitted with a stirrer
  2. temperaturereflux condensor
  3. additionis added
  4. temperatureheated to 150° C. for 4 hours
  5. temperatureThe mixture is then cooled to 80° C.
  6. temperatureWhen cooled to room temperature the crude
  7. customdye is separated by filtration, water and alcohol
  8. washwashed
  9. customdried overnight
  10. customaffords the pure helichromic compound