HRID980422
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
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
- temperaturethe reaction mixture is heated on a boiling waterbath for 13 hours
- additionhave been added
- custom3-β-aminoethylamino-4-nitrophenol hydrochloride crystallises
- filtrationIt is filtered off with suction
- washwashed with an ice-cold 2N hydrochloric acid solution
- customAfter recrystallisation from water
- customat a temperature above 260° C.