HRID562572

反应详情

EQUATION

反应方程式

HRID 562572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9.1 ml (0.13 mol) of 65% nitric acid are added dropwise in the course of 5 minutes to a yellow suspension of 20.0 g (0.13 mol) of 2-amino-4-nitrotoluene in 50 ml of absolute ethanol. When the exothermic reaction has subsided, 8.32 g (0.198 mol) of cyanamide dissolved in 8.3 ml of water are added. The brown reaction mixture is boiled at reflux for 25 hours, cooled to 0.degree. and filtered. Washing with 4.times.100 ml of ethanol/diethyl ether (1:1) and drying yield 2-methyl-5-nitrophenyl-guanidine nitrate; m.p. 219° C.-226° C.

WORKUP

后处理

  1. customWhen the exothermic reaction
  2. additionare added
  3. temperatureat reflux for 25 hours
  4. temperaturecooled to 0.degree
  5. filtrationand filtered
  6. washWashing with 4.times
  7. dry with material100 ml of ethanol/diethyl ether (1:1) and drying