HRID1077554

反应详情

EQUATION

反应方程式

HRID 1077554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 25.2 g (120 mmol) of 3-(1,1,2,2-tetrafluoroethoxy)aniline in 125 ml of ethanol are added 10.1 g (240 mmol) of cyanamide (50% in water). Then 16.3 ml (192 mmol) of concentrated hydrochloric acid are added to the brown solution and the mixture is refluxed for 19 hours. After cooling to room temperature, the reaction mixture is concentrated under reduced pressure and the residue is dissolved in 80 ml of water. After addition of 19.2 g (240 mmol) of ammonium nitrate, the product is isolated. by filtration, washed with water and dried at 60° C. under HV, giving 3-(1,1,2,2-tetrafluoroethoxy)phenylguanidine nitrate; m.p. 132°-134° C.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 19 hours
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. dissolutionthe residue is dissolved in 80 ml of water
  4. customthe product is isolated
  5. filtrationby filtration
  6. washwashed with water
  7. customdried at 60° C. under HV