Technetium-99m ( 99m Tc) is one of the most frequently used nuclides for single-photon emission computed tomography (SPECT) imaging because of its radiochemical characteristics, such as gamma emission of suitable energy (141 keV) and adequate half-life (6.01 h). Although triaquatricarbonyl 99m Tc cation ([ 99m Tc(CO) 3 (H 2 O) 3 ] + ) has several advantages as a 99m Tc-labeling agent, e.g., compact chelate size, chelate stability, and simplicity of preparation, its synthetic protocols should be improved. Because microwave heating is a convenient method for synthetic reactions, we studied the effect of microwave irradiation on the synthesis of 99m Tc tricarbonyl complexes. We found several factors beneficial for the preparation of nuclear medicines. In particular, microwave heating promoted one-pot syntheses of 99m Tc tricarbonyl chelates in a short time. In addition, the 99m Tc tricarbonyl complex could be obtained using low concentrations of ligands.