Synthesis
In a 100 ml flask, diethanolamine (10 g) was dissolved in chloroform (40 ml), and a chloroform (20 ml) solution of dichlorosulfoxide (2.6 ml) was added slowly and dropwise at room temperature. Reacted for 7h, the reaction was complete, spun dry, chloroform was added additionally, spun dry again and the dichlorosulfoxide was evaporated to dryness. It was dried to give 14 g of white solid (-chloroethyl)amine hydrochloride in 85% yield, mp: 214.1-215.2C (literature value > 215-216C).
1.58g (10mmol) of IX was added to 10ml of n-butanol with 1mol of aniline derivative and reacted at 180C for 30min in microwave. at the end of the reaction it was allowed to stand and cooled to precipitate crystals. The filter cake was washed with a small amount of dichloromethane and dried under vacuum to obtain white crystals of 1-(3-methylphenyl)piperazine dihydrochloride in 45-54% yield.
