An improved synthesis of (H/sub 2/EDTA)Tc(EDTAH/sub 2/) . 5H/sub 2/O

A new procedure for the preparation of the dimeric technetium complex (H/sub 2/EDTA)Tc(μ-O)/sub 2/Tc(EDTAH/sub 2/)-5H/sub 2/O,/sup 1/ has been developed. In the original preparation of this complex, HTcO/sub 4/, NaHSO/sub 3/, and EDTA were heated at 700C for several days and a crude product isolated by separating out crystals from a reaction mixture that had been allowed to evaporate very slowly. Analysis of the time course of this reaction shows that a reduced, presumably Tc(III), gold complex forms rapidly and that the prolonged reaction time is required only to decompose excess reducing agent and to oxidize the gold compound to the desired red product 1. The authors have found that careful oxidation of this gold complex with peroxide, followed by the addition of dilute HC1O/sub 4/, precipitates high yields of the sparingly soluble free acid form of 1 from the reaction mixture. The synthesis requires 24 hours, rather than several days