This research describes the synthesis of the commercially unavailable isomeric heptanone, 3,4-dimethyl-2-pentanone by reacting 2,3-dimethylbutanoic acid with lithium hydride to form lithium 2,3-dimethylbutanecarboxylate and treating the carboxylate product with methyllithium followed by aqueous acid. GC-Mass Spectral data of the product of synthesis as well as that of the product of synthesis after undergoing deuterium exchange confirmed that the product synthesized was 3,4-dimethyl-2-pentanone. The successful synthesis of 3,4-dimethyl-2-pentanone extends our micro-scale deuterium exchange GC-MS experiment in the organic chemistry laboratory.