| 3,4-二(吡嗪-2′-基)氧化呋咱的合成与表征 |
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| 引用本文： | 李亚南,张志忠,周彦水,陈斌,王伯周.3,4-二(吡嗪-2′-基)氧化呋咱的合成与表征[J].火炸药学报,2009,32(6). |
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| 作者姓名： | 李亚南 张志忠 周彦水 陈斌 王伯周 |
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| 作者单位： | 西安近代化学研究所,陕西,西安,710065 |
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| 摘 要： | 以2-氰基吡嗪为原料,经肟化、重氮化、脱氮、环化四步反应合成出-3,4-二(吡嗪-2′-基)氧化呋咱(DPF),总收率为51.0%,纯度99.3%;利用红外光谱、核磁共振、质谱、元素分析等手段对中间体与目标化合物的结构进行表征;探讨了氧化呋咱成环反应机理以及肟化、重氮化/脱氮及氧化呋咱成环的影响因素.氧化呋咱成环的最佳反应条件:Na_2CO_3摩尔量为理论值的1.10～1.25倍,反应温度2～10℃,反应时间4 h,收率75.6%,纯度不小于99.0%(HPLC).
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| 关 键 词： | 有机化学 有机合成 4-二(吡嗪-2′-基)氧化呋咱 表征 3 4-bis(pyrazine-2′-yl)furoxan |
Synthesis and Characterization of 3,4-Bis(pyrazine-2′-yl)furoxan |
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| LI Ya-nan,ZHANG Zhi-zhong,ZHOU Yan-shui,CHEN Bin,WANG Bo-zhou.Synthesis and Characterization of 3,4-Bis(pyrazine-2′-yl)furoxan[J].Chinese Journal of Explosives & Propellants,2009,32(6). |
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| Authors: | LI Ya-nan ZHANG Zhi-zhong ZHOU Yan-shui CHEN Bin WANG Bo-zhou |
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| Abstract: | 3,4-Bis(pyrazine-2′-yl)furoxan(DPF) was synthesized using 2-cyanopyrazine as raw material, via four-step reactions of oxime, diazotization, denitrification and cyclization and the overall yield was 51.0%. The structures of target compound and intermediates were characterized by IR, NMR, MS and elemental analysis. The mechanism of cyclization reaction was investigated. The affecting factors of reactions were optimized. The optimum reaction conditions of cyclization were: molar ratio n_(exp)∶n_(theory)=1.10-1.25 for Na_2CO_3, reaction temperature 2 to 10℃ and reaction time 4 h. The yield of DPF is about 75.6% and purity 99.0%. |
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| Keywords: | 3 DPF organic chemistry organic synthesis DPF characterization |
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