【摘要】 以二氨基呋咱(DAF)为起始原料,经Caros acid氧化、锌粉还原、环化、缩合和硝化五步反应得到N,N′-二硝基-N,N′-二(3-([1,2,3]-三唑并[4,5-c]呋咱-4,5-内盐-5-基)呋咱-4-基)二氨基甲烷(MNOTO),总收率为32.7%(以DAF计)。用元素分析、核磁共振、红外光谱等进行了结构表征。用浓硝酸和醋酐作为硝化体系硝化N,N′-二(3-([1,2,3]-三唑并[4,5-c]呋咱-4,5-内盐-5-基)呋咱-4-基)二氨基甲烷(MAOTO),考察了反应温度、反应时间以及浓硝酸与醋酐摩尔比对反应收率的影响,硝化体系中硝酸和醋酐的最佳摩尔比为1.5∶1,反应温度15～20℃,反应时间为5h。更多还原

【Abstract】 Starting from diaminofurazan(DAF),5,5′-[methanedinitramino-bis(1,2,5-oxadiazol-4,3-diyl)]bis[1H-triazolo-oxadiazolium]-bis(innersalt)(MNOTO) was synthesized by oxidation with Caro′s acid,reduction with Zn dust,cyclization,condensation reaction and nitration with condense nitrate acid/acetic anhydride in 32.7% yield.The structures of intermediates and MNOTO were characterized by elemental analyses,IR and NMR.Condense nitrate acid with acetic anhydride was employed in the nitration of 5,5’-[Methanediamino-bis(1,2,5-oxadiazol-4,3-diyl)]bis[1H-triazolooxadiazolium]-bis(innersalt)(MAOTO).The effects of reaction temperature,reaction time and molar ratio of condense nitrate acid to acetic anhydride on the conversion of MAOTO to MNOTO were studied.The optimal reaction conditions obtained were:reaction temperature,15-20℃;reaction time,5 h;the molar ratio of condense nitrate acid to acetic anhydride,1.5∶1.更多还原