The reaction of Pi-hydroxyphthalimide with w, w'-dibromoalkanes yields w-(phthalimido6xy) alkyl bromides, Ia, and w, w'-bis (phthalimidooxy) alkanes, Ib. Reaction of Ia with thiourea, followed by hydrolysis, leads to a facile synthesis of S-[w-(aminooxy) alkyl] isothiuronium salts, IIc. Hydrolysis of Ib makes available w, w'-bis (amino-0xy) alkanes which were characterized by their salts, amide and sulfonamide derivatives.