Our main goal was to form various compounds of the chloroacetylation product of p-methoxyphenol (4-methoxyphenyl 2-chloroacetate) with various amines using the Menshutkin reaction. This article presents a part of our research, namely, the reaction process with 2,4-dinitrophenyl hydrazine and its analysis. The process was carried out in different solvents. The expected product of the reaction was 2-(2,4-dinitrophenyl)-1-(2-(4-methoxyphenoxy)-2-oxoethyl)hydrazin-1-ium chloride. Due to regrouping, another product was formed. As a result of our research, 2,4-dinitrophenylhydrazide of monochloroacetic acid (2-chloro-N'-(2,4-dinitrophenyl)acetohydrazide) was formed. Crystal structure analysis was performed. This is of interest because of its potential applications in various fields, including pharmaceuticals and materials science. The synthesis of the compound was achieved by a direct synthetic route and confirmed by spectroscopic methods such as IR, NMR, and elemental analysis. Single-crystal X-ray diffraction analysis provided detailed structural information, revealing the molecular arrangement within the crystal lattice. Crystallographic data revealed a monoclinic crystal system with the space group P21/n, which revealed the molecular conformation, intermolecular interactions, and crystal packing motifs. This comprehensive structural characterization enhances our understanding of the compound's properties and provides valuable insights for further exploration of its potential applications. As a result, a compound with a confirmed crystal structure was entered into the reference of Structures The Cambridge Crystallographic Data Centre (CCDC).