1,4,5,8-四硝基-1,4,5,8-四氮杂双环[4.4.0]癸烷合成工艺的改进?

wf(2016)

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Abstract
为了改进1,4,5,8-四硝基-1,4,5,8-四氮杂双环[4.4.0]癸烷(TNAD)的合成方法,以1,4,5,8-四氮杂双环[4.4.0]癸烷(THAD)为原料,经成盐、硝化两步反应合成出了TNAD,反应总收率为90%,纯度为98.7%。采用红外光谱、核磁共振氢谱及元素分析对产品结构进行了表征。考察了硝化体系、物料比、反应温度、反应时间对硝化反应的影响,确定了最佳的反应条件:n(THAD.4HNO3)︰ n(98%HNO3)︰n(AC2O)=1︰24︰15,反应温度为25℃,反应时间为2 h。
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Key words
organic chemistry,8-tetranitro-1,8-tetraazabicyclo [4. 4. 0]decalin (TNAD),salt-forming reaction,nitrolysis,HNO3/AC2 O
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