Synthetic routes to 3-alkylidene-2, 5-piperazinedione have been studied. An enamine carboxylate, methyl 2-amino-3-methyl-2-butenoate, was treated with phthaloylglycyl chloride to give methyl 3-methyl-2-phthaloylglycylamino-2-butenoate, which, after removal of phthaloyl group, was cyclized to yield 3-isopropylidene-2, 5-piperazinedione. The condensation reaction of the piperazinedione with aromatic aldehydes was also studied, ...