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作 者:董琳琳[1] 张光全[2] 池钰[2] 范桂娟[2] 何玲[1] 陶国宏[1] 黄明[2]
机构地区:[1]四川大学化学学院,四川成都610064 [2]中国工程物理研究院化工材料研究所,四川绵阳621900
出 处:《含能材料》2012年第6期690-692,共3页Chinese Journal of Energetic Materials
基 金:国家自然科学基金(21103116)
摘 要:以乙二醛和盐酸羟胺为原料,合成了二氨基乙二肟(DAG),经过脱水成环得到3,4-二氨基呋咱(DAF),再在30%的双氧水作用下氧化得到亚硝基氨基呋咱(ANF),ANF与N,N-二溴叔丁基胺缩合得到3-氨基-4-(叔丁基氧化偶氮基)呋咱,最后经四氟硼酸銷(NO2BF4)硝化成环得目标产物FTDO,总收率18%(基于DAF),并对其进行了红外和核磁表征。Furazano[3,4-e]-1,2,3,4-tetrazine-1 ,3-dioxide(FTDO) has been synthesized in the work. Firstly, diaminoglyoxime (DAG) was obtained via the one-step reaction of glyoxal with hydroxylammonium chloride. 3,4-Diaminofurazan(DAF) was obtained by the dehydration reaction of DAG. Then the oxidation of DAF using 30% H2O2 gave 3-amino-4-nitrosofurazan(ANF) , and 3-amino-4-(tert-butyl)azoxyfurazan was prepared after the treatment of ANF with tert-butyI-N,N-dibromide in dichloromethane. Finally, FTDO was obtained by the nitration and cyclization of 3-amino-4-(tert-butyl)azoxyfurazan with nitronium tetraflu-orobrate ( NO,BF4 ) in acetonitrile with the total yield of 18%,. The structures of FTDO and its intermediates were characterized by IR and NMR.
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