HRID1077554
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture is refluxed for 19 hours
- concentrationthe reaction mixture is concentrated under reduced pressure
- dissolutionthe residue is dissolved in 80 ml of water
- customthe product is isolated
- filtrationby filtration
- washwashed with water
- customdried at 60° C. under HV