HRID980422

反应详情

EQUATION

反应方程式

HRID 980422 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 mixture is heated on a boiling waterbath for 13 hours. The cooled solution is then poured into 2.6 liters of ice-water to which 1.09 liters of hydrochloric acid (d=1.18) have been added. After the mixture has been cooled to -10° C. for a few hours, 3-β-aminoethylamino-4-nitrophenol hydrochloride crystallises. It is filtered off with suction and washed with an ice-cold 2N hydrochloric acid solution 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 mixture is heated on a boiling waterbath for 13 hours
  2. additionhave been added
  3. custom3-β-aminoethylamino-4-nitrophenol hydrochloride crystallises
  4. filtrationIt is filtered off with suction
  5. washwashed with an ice-cold 2N hydrochloric acid solution
  6. customAfter recrystallisation from water
  7. customat a temperature above 260° C.