3,4-双(3'-氨基呋咱-4'-基)呋咱的合成与表征

Synthesis and Characterization of 3,4-Bis-(3′-aminofurazal-4′-yl)-furazan(BATF)

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SnC l2/HC l/AcO H,料比n(还原剂)n(DAT F)为31～41,反应温度为75℃,时间为7 h。

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（EI） 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.