HRID2155

反应详情

EQUATION

反应方程式

HRID 2155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.3 g (150 mmol) of cyanamide (50% in water) are added to a suspension of 16.1 g (100 mmol) of 3-trifluoromethyl-aniline in 35 ml of ethanol. 7.0 ml of nitric acid (65%, 0.1 mol) are then added to the brown solution and the reaction mixture is heated for 20 h under RF. It is then cooled to 0° and filtered, and the material retained on the filter is washed with ethanol and dried at 60° under HV to give 3-trifluoromethyl-phenylguanidine nitrate; 1H-NMR (dimethyl sulfoxide): 7.6 (7H,m), 9.9 (1H,br,s).

WORKUP

后处理

  1. temperaturethe reaction mixture is heated for 20 h under RF
  2. temperatureIt is then cooled to 0°
  3. filtrationfiltered
  4. washis washed with ethanol
  5. customdried at 60° under HV