Three new hydrazones were synthesized by condensation reaction between 3,4-dimethoxy-2-nitrobenzaldehyde and aryl hydrazine hydrochlorides. 3,4-Dimethoxy-2-nitrobenzaldehyde needed for the Schiff base-imine condensation reaction was synthesized from vanillin through esterification, nitration, hydrolysis, and methylation reactions. All products were purified by re-crystallization in a suitable solvent. The structures of three new hydrazones were determined by 1H NMR, 13C NMR, and MS.