AbstractMethods described in the literature are inadequate for the preparation of pure polyethylene glycol (PEG) tosylate. Therefore an improved method is presented. The hydroxyl groups on PEG can be quantitatively converted into the tosylate and isolated from the reaction medium free from impurities with no chain cleavage or reduction in molecular weight. 1,2‐Di(N‐phenyl 2‐aminoethoxy) ethane, α,ω‐di(N‐phenyl 2‐aminoethyl) poly(oxyethylene), and α,ω‐di(N‐phenyl,N‐benzyl 2‐aminoethyl) poly(oxyethylene) were prepared from the tosylates of tri‐ and poly(ethylene glycol)s and the corresponding primary and