3,4-双(3'-氨基呋咱-4'-基)呋咱的合成与表征

摘要

以3-氨基-4-酰氯肟基呋咱(AAOF)为原料,经分子间二聚生成3,4-二氨基呋咱基氧化呋咱(DATF),DATF还原生成了新化合物3,4-双(3’-氨基呋咱-4’-基)呋咱(BATF),总收率为54％,采用红外光谱、核磁共振光谱、质谱、元素分等进行了结构表征.通过质谱裂解碎片,研究了BATF的碎裂反应机理；探讨了还原反应关键影响因素,确定了最佳的反应条件为:还原剂为SnCl2/HCl/AcOH,料比n(还原剂)∶n(DATF)为3∶1～4∶1,反应温度为75℃,时间为7h.%A novel energetic material 3,4-bis-(3'-aminofurazal-4'-yl)-furazan(BATF) was synthesized with yield of 54％ using reduction of 3,4-bis-(3'-aminofurazal-4'-yl)-furoxan (DATF) and DATF was produced by dimerization of 3-aninofurazan-4-carboxchlorid-oxime(AAOF).Its structure was characterized by IR,13C NMR,1H NMR,MS and elemental analysis.The split mechanism of BATF was investigated by MS(El) spectra analysis.The synthetic conditions of reduction were optimized as follows:SnCl2 ·2H2O is reductant in the mixed water solution of HCl and AcOH,n(SnCl2 · 2H2O) ∶ n(DATF)is 3 ∶ 1 ～4 ∶ 1,the reaction temperature 75 ℃ and the reaction time 7 h.