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含能材料  2014 

2,2,4,4-四硝基金刚烷的合成与表征

DOI: 10.3969/j.issn.1006-9941.2014.04.004

Keywords: 有机化学,2,2,4,4-四硝基金刚烷,金刚烷酮,合成,硝化,五氧化二氮

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Abstract:

以金刚烷酮为原料,经Baeyer-Villiger氧化、内酯重排、缩酮化、氧化和偕硝化等单元反应合成了2,2,4,4-四硝基金刚烷。优化了重要中间体4,4-乙撑二氧基金刚烷-2-酮的合成方法。使用绿色硝化剂五氧化二氮对酮肟进行偕硝化反应,考察了溶剂、温度、反应时间、物料配比对第一步偕硝化反应的影响,确定了最佳反应条件:溶剂为二氯甲烷,n(4,4-乙撑二氧基-2-金刚烷酮肟)∶n(五氧化二氮)=1∶3,反应温度为45℃,反应时间为30min,收率为52.3%。本路线总收率为14.2%,是文献报道的2.9倍。

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