Bis(2-chloroethyl)amine → 1-(3,5-difluorophenyl)piperazine hydrochloride

Participants

Reaction Steps

13.7 g of bis-(2-chloroethyl)amine was suspended in 120 ml of butanol. To the obtained solution was added 10 g of 3,5-difluoroaniline and the mixture was heated under reflux for 48 hours. After cooling, 10.6 g of potassium carbonate was added and the obtained mixture was heated under reflux for additional 24 hours. Then crystals were collected by filtration, dissolved in water, extracted with chloroform, successively washed 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 and converted into hydrochloride by adding a 4N hydrochloric acid/dioxane solution. After filtration, 12.6 g of the title compound was obtained.

Provenance & Evidence