Technetium-99m diethyldithiocarbamate (99mTc-DDC) was prepared by reduction of [99mTc]pertechnetate with formamidine sulfinic acid in the presence of DDC at alkaline pH, both from extemporaneous solutions and in a kit formulation. The properties of 99mTc-DDC were compared in vitro and in vivo with those of 201Tl-DDC, an agent used for cerebral perfusion imaging (CPI). 99mTc-DDC is a lipophilic complex but its oil/water partition coefficient is lower than that of 201Tl-DDC. 99mTc-DDC also shows greater binding to plasma proteins. Studies in rabbits show that 99mTc-DDC enters the brain but is not retained to the same extent as 201Tl-DDC. This lack of retention may be because 99mTc-DDC does not decompose rapidly in lipid media as 201Tl-DDC does. These results suggest that 99mTc-DDC in its present formulation is not suitable for CPI with SPECT.