HRID637586

反应详情

EQUATION

反应方程式

HRID 637586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 11.1 g (40 mmol) of 1,5-dichloro-9,10-anthracenedione, 13.1 g (110 mmol) of 2-[(hydrazinoethyl)amino]ethanol, 4 g of anhydrous potassium bicarbonate, 1 g of anhydrous potassium fluoride, and 110 ml of dimethyl sulfoxide is stirred at 70° C. overnight. The mixture is chilled and the solids are collected by filtration, washed with water, then thoroughly with acetonitrile to give a residue that is crystallized from 2-propanol to leave 2.6 g of product. The hydrochloride salt is prepared as described in Example 3; mp 272°-273° C. (decomposition).

WORKUP

后处理

  1. temperatureThe mixture is chilled
  2. filtrationthe solids are collected by filtration
  3. washwashed with water
  4. customthoroughly with acetonitrile to give a residue that
  5. customis crystallized from 2-propanol