A series of 99mTc-bis(aminoethanethiol)-fatty acid (99mTc-BAT-fatty acid) analogs were synthesized and evaluated as potential tracers of myocardial metabolism. The BAT-fatty acid precursors were prepared using a new synthetic route that avoids the use of strong reducing agents such as lithium aluminum hydride. Biodistribution studies of the no-carrier-added 99mTc-complexes were conducted in rats using [125I]IPPA as an internal standard. The myocardial uptake of the 99mTc-BAT-fatty acid analogs was significantly less than that of [125I]IPPA and indicates the 99mTc analogs are not suitable candidates for SPECT-based myocardial imaging studies.