The present work refers to the synthesis of novel dialkylacylphosphonylhydrazones that occurs in three reaction steps: the first one is the synthesis of different dialkyl acetate phosphonoacetates obtained by the reaction of ethyl bromoacetate with the trialkyl phosphite of interest. The second one is the synthesis of acetic diethoxyphosphonylhydrazines which is from the reaction between the synthesized dialkyl phosphonoacetates and hydrazine. The third and final steps is the condensation of acetic diethoxyphosphonylhydrazides with different heterocyclic aldehydes. In total, 17 unpublished compounds, namely 1 to 17 (Table 1) were obtained with a diastereoisomeric mixture of the preferential conformation E and all the compounds were characterized by 1-H and 13-C and 31-P NMR, infrared (IR) and mass spectroscopy (MS). This work presents the characterization data of these compounds.