反应详情

10.1 g (240 mmol) of cyanamide (50% in water) are added to a suspension of 25.2 g (120 mmol) of 3-(1,1,2,2-tetrafluoro-ethoxy)-aniline in 125 ml of ethanol. 16.3 ml of hydrochloric acid (conc., 192 mmol) are then added to the brown solution and the reaction mixture is heated under reflux for 19 h. After cooling to RT, the reaction mixture is concentrated under reduced pressure and the residue is dissolved in 80 ml of water. After the addition of 19.2 g (240 mmol) of ammonium nitrate, the product is isolated by filtration, then washed with water and dried at 60° under I-HV. 3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl-guanidine nitrate is obtained; m.p. 132°-14133°.

1. temperaturethe reaction mixture is heated
2. temperatureunder reflux for 19 h
3. concentrationthe reaction mixture is concentrated under reduced pressure
4. dissolutionthe residue is dissolved in 80 ml of water
5. customthe product is isolated by filtration
6. washwashed with water
7. customdried at 60° under I-HV