HRID1730999

反应详情

EQUATION

反应方程式

HRID 1730999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1.4 Grams of a palladium on carbon catalyst was added to a mixture of 154 grams of 5-nitrotetrahydroanthraquinone and 3000 grams of methyl cellosolve, into which was fed hydrogen at room temperature under normal pressure for hydrogenation. After hydrogen was absorbed in an amount of 2 mols per mol of the 5-nitro compound, the catalyst was separated by filtration. To the resultant filtrate was added 60 grams of triethylamine, followed by agitating at 100° C. for 3 hours and feeding air at 100° C. for 1 hour. Then, methyl cellosolve was removed by distillation until crystals began to precipitate. The solution was allowed to cool and the crystals were separated by filtration, washed with water and dried to obtain 118 grams of 1-aminoanthraquinone having a purity of 98.0%.

WORKUP

后处理

  1. customat room temperature
  2. customAfter hydrogen was absorbed in an amount of 2 mols per mol of the 5-nitro compound
  3. customthe catalyst was separated by filtration
  4. additionTo the resultant filtrate was added 60 grams of triethylamine
  5. customat 100° C.
  6. customfor 1 hour
  7. customThen, methyl cellosolve was removed by distillation until crystals
  8. customto precipitate
  9. temperatureto cool
  10. customthe crystals were separated by filtration
  11. washwashed with water
  12. customdried