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The first 2-nitrodiazene 1-N-oxides were synthesized at the N.D. Zelinsky Institute of Organic Chemistry. A synthetic approach to these compounds includes the nitration of 2-(tert-butyl)-diazene 1-N-oxides. The plausible mechanism for the synthesis of 2-nitrodiazene 1-N-oxides involves the formation of a cationic intermediate A followed by elimination of the tert-butyl cation. The nitrodiazene oxide group has been scarcely studied and has recently attracted much attention. There is little information available concerning thermal stability of 2-nitrodiazene 1-N-oxides. In order to assess the applicability of 2-nitrodiazene 1-N-oxides as high energy compounds, it is important to scrutinize its thermal stability. Methods for the synthesis of novel energetic materials based on furazan cycle and nitrodiazene oxide group have been developed. 3-Amino-4-(tert-butyl-NNO-azoxy)furazan is a starting material for the synthesis of target compounds. The compounds obtained are relatively thermally stable. 3-Nitro-4-{[4-(nitro-NNO-azoxy)furazan-3-yl]-NNO-azoxy}furazan was found to be the most stable (Tonset = 115 °C). Its structure was studied by X-ray diffraction. These compounds could be considered as energetic materials.