99mTc hexakis (2-methoxyisobutylisonitrile) is a cationic complex useful as a myocardial perfusion agent. The synthesis of 2-methoxyisobutylisonitrile (MIBI) by a modified and improved procedure in a two-step process with an overall yield of 53% is described. The preparation of its copper and technetium-99m complexes is also presented.