Abstract: A process for preparing S-(&ohgr;-aminoalkylamino) alkyl aryl sulfide dihydrochlorides includes the steps of (a) reacting aryl mercaptan and (&ohgr;-aminoalkylamino) alkylbromide dihydrobromide to cause condensation thereof in the presence of an organic base in an organic solvent and provide a condensation product; (b) converting the condensation product to a dihydrochloride salt; and (c) precipitating the dihydrochloride salt. Preferably the precipitated dihydrochloride salt is recrystallized. These dihydrochlorides are new and effective antidotes for sulfur mustard toxicity.