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2-氨基-6-羟基-3,5-二硝基吡啶的合成探索
引用本文:叶福达,金宁人,刘浩杰,张清义. 2-氨基-6-羟基-3,5-二硝基吡啶的合成探索[J]. 化工进展, 2015, 34(4): 1098-1103,1114. DOI: 10.16085/j.issn.1000-6613.2015.04.034
作者姓名:叶福达  金宁人  刘浩杰  张清义
作者单位:浙江工业大学化学工程学院, 浙江 杭州 310032
基金项目:江苏省科技支撑计划(BE 2011129);浙江省教育厅科研(Y201121211)项目
摘    要:2-氨基-6-羟基-3,5-二硝基吡啶(AHDNP)是合成聚对苯亚乙基吡啶并咪 二唑(PPIO)重要前体.本文以2,6-二氯吡啶为原料经单硝化、单氨解、再硝化先合成中间体2-氨基-6-氯-3,5-二硝基吡啶(ACDNP),纯度为95.60%,总收率41.00%以上;最后在K2CO3的碱性水溶液中70℃条件下单水解,成功合成出AHDNP,提纯后总收率为82.07%,纯度为98.13%.AHDNP的结构经过FT-IR、MS、13C NMR 准确定性和表征.合成过程操作方便、产品质量优异、经济性良好及易于产业化,为进一步研发合成新型高性能材料PPIO及其新单体提供技术基础及中间体来源.

关 键 词:2-氨基-6-羟基-3  5-二硝基吡啶  2-氨基-6-氯-3  5-二硝基吡啶  2  6-二氯-3-硝基吡啶  聚对苯亚乙基吡啶并咪二唑  水解  合成  
收稿时间:2014-09-24

Synthesis of 2-amino-6-hydroxy-3,5-dinitropyridine
YE Fuda , JIN Ningren , LIU Haojie , ZHANG Qingyi. Synthesis of 2-amino-6-hydroxy-3,5-dinitropyridine[J]. Chemical Industry and Engineering Progress, 2015, 34(4): 1098-1103,1114. DOI: 10.16085/j.issn.1000-6613.2015.04.034
Authors:YE Fuda    JIN Ningren    LIU Haojie    ZHANG Qingyi
Affiliation:College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310032, Zhejiang, China
Abstract:As a key intermediate for poly (p-phenylene-2-pyridinoimidazol-6-oxazole),2-amino-6- chloro-3,5-dinitropyridine(ACDNP) with 95.60% and the total yield of 41% was obtained from 2,6-dichloropyridine by nitration,ammonolysis and nitration. 2-Amino-6-hydroxy- 3,5-dinitropyridine (AHDNP) was prepared from ACDNP in potassium carbonate solution at 70℃. The purity of AHDNP was 82.07% and the total yield of AHDNP is 98.13% after re-crystallization. AHDNP was identified by FT-IR,MS and 13C NMR. This process for AHDNP synthesis has advantages of simple operation procedure,excellent product quality,good economy and easy industrialization etc.,which provides convenience for further development of PPIO and other high-performance materials.
Keywords:2-amino-6-hydroxy-3,5-dinitropyridine  2-amino-6-chloro-3,5-dinitropyridine  2,6- dichloro-3-nitropyridine  ploy(p-phenylene-2-pyridoimidazol-6-oxazole)(PPIO)  hydrolysis  synthesis
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