反应详情

4.12 ml (39.12 mmol) of 3-chloro-aniline are placed in 25 ml of ethanol, and 3.3 g (78.4 mmol) of cyanamide are added. 5.3 ml (62.7 mmol) of concentrated hydrochloric acid are added dropwise to the brown solution. The reaction solution is then stirred for 20 hours at 78°. After concentration under reduced pressure, the residue is dissolved in 25 ml of water, and 6.3 g (78.4 mmol) of ammonium nitrate are added. The precipitated substance is isolated by filtration, washed with water and dried at 60° under HV. 3-chloro-phenyl-guanidine nitrate is obtained; 1H-NMR (dimethyl sulfoxide): 7.2-7.8 (7H,m), 9.9 (1H,br,s).

1. concentrationAfter concentration under reduced pressure
2. dissolutionthe residue is dissolved in 25 ml of water
3. customThe precipitated substance is isolated by filtration
4. washwashed with water
5. customdried at 60° under HV