HRID647784
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionA suspension of 3.11 g
- temperatureheated
- temperatureunder reflux
- distillationof water is collected as distillate over a 3 hour period, with no additional water after a total of 7 hours
- temperatureof refluxing
- filtrationThe hot solution is filtered
- customremoving a small amount of blue-black solid
- concentrationThe filtrate is concentrated
- additionpetroleum ether is added
- customto give a gum which
- customThe solid is collected
- washwashed with benzene
- customto give 2.05 g