HRID1494283

反应详情

EQUATION

反应方程式

HRID 1494283 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

0.432 mol (75 g) of 3-chloro-4-nitrophenol is introduced into 282 ml of ethylenediamine and the reaction medium is then heated in a boiling water-bath for 13 hours. The cooled solution is then poured into 2.6 liters of iced water to which 1.09 liters of hydrochloric acid (d=1.18) has been added. After cooling at -10° C. for a few hours, the 3-β-aminoethylamino-4-nitrophenol hydrochloride crystallises. It is filtered off and washed with an ice-cold 2N solution of hydrochloric acid and then with ethanol. After recrystallisation from water, the dried product melts with decomposition at a temperature above 260° C.

WORKUP

后处理

  1. temperaturethe reaction medium is then heated in a boiling water-bath for 13 hours
  2. additionhas been added
  3. customthe 3-β-aminoethylamino-4-nitrophenol hydrochloride crystallises
  4. filtrationIt is filtered off
  5. washwashed with an ice-cold 2N solution of hydrochloric acid
  6. customAfter recrystallisation from water
  7. custommelts with decomposition at a temperature above 260° C.