1,2,4-Triazoles, as heterocyclic compounds, represent an attractive class of ligands in the design of metal–organic frameworks (MOFs) due to their donor–acceptor character, thermal and chemical stability, and ability to form extended coordination networks. This review summarizes the literature published between 2019 and 2025 on luminescent MOFs incorporating 1,2,4-triazole scaffold. The analysis covers synthetic conditions and provides a detailed discussion of the luminescent properties of these materials. Particular emphasis is placed on their applicability as luminescent probes for environmental monitoring and medical diagnostics, as well as on their potential use in light-emitting diode construction. The collected data highlight promising results, including strong correlations between analyte concentration and luminescent response, enabling sensitive detection with low limits of detection (LOD) for selected analytes. This article may serve as a valuable resource for chemists, physicists, and engineers involved in the design of functional materials and the development of detection and optoelectronic technologies.

A series of new symmetrical 2,5-dialkyl-1,3,4-oxadiazoles containing substituted alkyl groups at the terminal positions with substituents, such as bromine, isopropyloxycarbonylmethylamino, and carboxymethylamino, were successfully synthesized. The developed multistep method employed commercially available acid chlorides differing in alkyl chain length and terminal substituent, hydrazine hydrate, and phosphorus oxychloride. The intermediate bromine-containing 2,5-dialkyl-1,3,4-oxadiazoles were easily substituted with diisopropyl iminodiacetate, followed by hydrolysis in aqueous methanol solution giving the corresponding 1,3,4-oxadiazoles bearing carboxymethylamino substituents. The structure of all products was confirmed by conventional spectroscopic methods including ¹H NMR, ¹³C NMR, and HRMS.