HRID1494283
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 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
- temperaturethe reaction medium is then heated in a boiling water-bath for 13 hours
- additionhas been added
- customthe 3-β-aminoethylamino-4-nitrophenol hydrochloride crystallises
- filtrationIt is filtered off
- washwashed with an ice-cold 2N solution of hydrochloric acid
- customAfter recrystallisation from water
- custommelts with decomposition at a temperature above 260° C.