4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo [5.5.0.0~(5,9)0~(3,11)]dodecane Synthesis

摘要

4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.0~(5,9)0~(3,11)]dodecane (TEX) was obtained by nitrolysis of l,4-diformyl-2,3,5,6-tetrahydroxypiperazine reaction using a mixture of fuming nitric acid and concentrated sulfuric acid The optimal process temperature was 54-56°C. The yield of the synthesis depends inter alia on the rate the reactants are introduced into the reaction medium and on the time of conditioning of the reaction mixture. A maximal yield of ca. 40% was achieved at the reactant addition time of 2h and conditioning time of 2h. None of the other nitrating mixtures examined proved superior to the conventional nitrating mixture. The product was examined by high-performance liquid chromatography (HPLC), nuclear magnetic resonance (NMR), Fourier transform infrared (FT1R), and differential scanning calorimetry (DSC) techniques and the results are reported