Condensation of 2,3-butanedione monooxime (I) with 2,2,-dimethyl-1,3-propanediamine (II) affords the bis-imine adduct (III). Subsequent reduction of the imine functions of (III) using NaBH4 in EtOH gives rise to a mixture of the meso-diamine (IV) and the racemic d,l-isomers (V). Separation of this mixture is achieved by either HPLC or fractional crystallization from acetonitrile and then from ethyl acetate. The target 99mtechnetium complex is prepared in situ by reduction of a solution of 99mTc-pertechnetate with stannous tartrate in the presence of the diamino dioxime ligand (V).