HRID65545

反应详情

EQUATION

反应方程式

HRID 65545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

120 parts of phenol, 6.1 parts (0.1 mole) of boric acid and 70 parts of toluene are refluxed, while stirring, the water of reaction formed thereby being removed from the system. The toluene is then distilled off, the mixture is cooled to 110° C. and 25.4 parts (0.05 mole) of 1-palmitylamino-8-amino-4,5-dihydroxyanthraquinone (prepared by reacting 1-amino-8-nitro-4,5-dihydroxyanthraquinone with palmityl chloride in nitrobenzene and then reducing the product with hydrazine hydrate) are added. Ammonia is then passed in at this temperature until no further starting material can be detected in the thin-layer chromatogram (duration: 3 hours). The reaction mixture is cooled to 90° C. and 240 parts of methanol are added. After cooling to room temperature, the dye precipitated is filtered off with suction and the material on the filter is washed with methanol and water and dried. 20 parts of 1,4-diamino-5-hydroxy-8-palmitylaminoanthraquinone of melting point 174° C. are obtained.

WORKUP

后处理

  1. customformed
  2. customthereby being removed from the system
  3. distillationThe toluene is then distilled off
  4. additionare added
  5. temperatureThe reaction mixture is cooled to 90° C.
  6. temperatureAfter cooling to room temperature
  7. customthe dye precipitated
  8. filtrationis filtered off with suction
  9. washthe material on the filter is washed with methanol and water
  10. customdried