HRID440870

反应详情

EQUATION

反应方程式

HRID 440870 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° and filtered. Washing with 4×100 mi of ethanol/diethyl ether (1:1) and drying yield 2-methyl-5-nitrophenyl-guanidine nitrate; m.p. 219°-226°.

WORKUP

后处理

  1. customWhen the exothermic reaction
  2. additionare added
  3. temperatureat reflux for 25 hours
  4. temperaturecooled to 0°
  5. filtrationfiltered
  6. washWashing with 4×100 mi of ethanol/diethyl ether (1:1)
  7. customdrying