HRID647784

反应详情

EQUATION

反应方程式

HRID 647784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 3.11 g. of 1,4-dihydroxy-5,8-bis[[2-(2-hydroxyethylamino)ethyl]amino]anthraquinone [prepared as described in Example 1(A)] in 55.0 ml. of benzene containing 2.02 g. of 2-furaldehyde is stirred and heated under reflux using a Dean-Stark trap. A total of 0.2 ml. of water is collected as distillate over a 3 hour period, with no additional water after a total of 7 hours of refluxing. The hot solution is filtered, removing a small amount of blue-black solid. The filtrate is concentrated and petroleum ether is added to give a gum which slowly solidifies. The solid is collected and washed with benzene to give 2.05 g. of a blue-black solid.

WORKUP

后处理

  1. additionA suspension of 3.11 g
  2. temperatureheated
  3. temperatureunder reflux
  4. distillationof water is collected as distillate over a 3 hour period, with no additional water after a total of 7 hours
  5. temperatureof refluxing
  6. filtrationThe hot solution is filtered
  7. customremoving a small amount of blue-black solid
  8. concentrationThe filtrate is concentrated
  9. additionpetroleum ether is added
  10. customto give a gum which
  11. customThe solid is collected
  12. washwashed with benzene
  13. customto give 2.05 g