A solution of 5 g of bis(3-methylsulfonyloxypropyl)amine hydrochloride in 20
ml of ice water is neutralized with 1N sodium carbonate solution. The resulting
amine base is extracted with five 20 ml portions of chloroform. The combined
extract is dried over anhydrous sodium sulfate, the solvent is distilled off
under reduced pressure, and the residue is dissolved in 20 ml of ethanol. To
the ethanol solution is added slowly with stirring under ice cooling a solution
of 2.6 g of p-toluenesulfonic acid in 30 ml of ethanol. The white precipitate
formed is collected by filtration and recrystallized from ethanol to give 5.0 g of
white crystalline bis(3-methylsulfonyloxypropyl)amine p-toluenesulfonate
melting at 115°C to 116°C.
