Synthesis of azoxytriazolone by electrochemical reduction of nitrotriazolone in wateritric acid system

摘要

3-nitro-1,2,4-triazol-5-one (NTO) is an important and prospective compound due to their reduced sensitivity for mechanical and shock initiation. Many derivatives of NTO are described in last years, especially salts and complexes. Nitrotriazolone is also valuable substrate for synthesis of azo- and azoxy compounds. We present the results of systematic study on electroreduction of NTO in distilled water (nitric acid was used as the electrolyte). Electrosyntheses were carried out using standard DC power supply with 12V voltage and 4A effective current maximum. Graphite electrodes with surface area of 160 cm~2 were used. Two series of experiments were conducted in laboratory scale. In the first tests reduction of NTO was conducted for 2-8 h with mechanical stirring. Next each experiment were repeated with additional stirring time (18 h) with no current. Solid products were collected by simple filtration, dried and weighed. The products were analyzed by using multinuclear NMR and DTA/TG techniques. Crystals shape were evaluated with images from optical microscope.