反应详情

7.0 g of bis(2-chloroethyl)amine hydrochloride was suspended in 60 ml of butanol and 5 g of 2,5-difluoroaniline was added thereto at room temperature. After heating under reflux for 72 hours, the reaction mixture was cooled and 4.1 g of sodium carbonate was added. After heating under reflux for additional 24 hours, the precipitate was taken up by filtration, dissolved in water and extracted with chloroform. Then the extract was washed successively with water and a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate. After evaporating the solvent, the residue was dissolved in a small amount of chloroform, converted into hydrochloride by adding a 4N hydrochloric acid/dioxane solution and filtered to thereby give 2.39 g mg of the title compound.

1. customat room temperature
2. temperatureAfter heating
3. temperatureunder reflux for 72 hours
4. temperaturethe reaction mixture was cooled
5. temperatureAfter heating
6. temperatureunder reflux for additional 24 hours
7. filtrationthe precipitate was taken up by filtration
8. dissolutiondissolved in water
9. extractionextracted with chloroform
10. washThen the extract was washed successively with water
11. dry with materiala saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate
12. customAfter evaporating the solvent
13. dissolutionthe residue was dissolved in a small amount of chloroform
14. additionby adding a 4N hydrochloric acid/dioxane solution
15. filtrationfiltered