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2,3,5,6-四氨基吡啶及其(2-羟基)对苯二甲酸复合盐的合成
引用本文:杨健,金宁人,张青龙,张清义.2,3,5,6-四氨基吡啶及其(2-羟基)对苯二甲酸复合盐的合成[J].化工进展,2014,33(6):1556-1562.
作者姓名:杨健  金宁人  张青龙  张清义
作者单位:浙江工业大学化工与材料学院,浙江 杭州 310032
基金项目:江苏省科技支撑计划项目(BE 2011129)
摘    要:为了制备高纯度与高收率的2,3,5,6-四氨基吡啶/2-羟基对苯二甲酸复合盐(TH盐),通过以2,6-二氨基-3,5二硝基吡啶(DADNP)为原料催化加氢还原制得2,3,5,6-四氨基吡啶盐酸盐(TAPH)。反应在55~60℃的氢气氛围下,以甲醇为溶剂,Pd/C为催化剂制得纯度99.4%的TAPH,收率82.1%。制成的盐酸盐再和2-羟基对苯二甲酸(HTA)钠盐在氮气氛围的保护下合成2,3,5,6-四氨基吡啶/2-羟基对苯二甲酸复合盐(TH盐)单体,结构经过13C-NMR、MS和FT-IR表征分析,结果表明是目的产物,纯度达98%以上。

关 键 词:2  3  5  6-四氨基吡啶/2-羟基对苯二甲酸复合盐(TH盐)  2  3  5  6-四氨基吡啶盐酸盐(TAPH)  2-羟基对苯二甲酸(HTA)  2  6-二氨基-3  5二硝基吡啶(DADNP)  2  3  5  6-四氨基吡啶/2-羟基对苯二甲酸复合盐  2  3  5  6-四氨基吡啶盐酸盐  2-羟基对苯二甲酸  2  6-二氨基-3  5二硝基吡啶  

Synthesis of 2,3,5,6-tetraaminopyridine and its 2-hydroxyterephthalic acid composite salt
YANG Jian;JIN Ningren;ZHANG Qinglong;ZHANG Qingyi.Synthesis of 2,3,5,6-tetraaminopyridine and its 2-hydroxyterephthalic acid composite salt[J].Chemical Industry and Engineering Progress,2014,33(6):1556-1562.
Authors:YANG Jian;JIN Ningren;ZHANG Qinglong;ZHANG Qingyi
Affiliation:College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou 310032,Zhejiang,China
Abstract:In order to prepare the composite salt of 2,3,5,6-tetraaminopyridine and 2-hydroxyterephthalic acid (TH salt) with high purity and yield,the 2,3,5,6-tetraaminopyridine hydrochloride(TAPH) was successfully reduced by catalytic hydrogenation from 3,5-dinitropyridine- 2,6-diamine(DADNP) as raw material. TAPH was obtained with the purity of 99.4% and the yield of 82.1% in hydrogen and 55~60℃ condition,the solvent is methanol and the catalyst is Pd/C. Under the protection of the nitrogencondition,the TAPH and 2-hydroxyterephthalic acid(HTA) sodiumsalt were taken as raw materials to make the composite salt of 2,3,5,6-tetraaminopyridine with 2-hydroxyterephthalic acid(TH salt). All chemical structures of the products were identified by 13C-NMR,MS and FT-IR,the result showed that the product was the aim product and its purity was up to 98%.
Keywords:2  3  5  6-tetraaminopyridine/2-hydroxyterephthalic acid composite salt (TH salt)  2  3  5  6-tetraaminopyridine hydrochloride(TAPH)  2-hydroxyterephthalic acid(HTA)  3  5-dinitropyridine-2  6-diamine(DADNP)  2  3  5  6-tetraaminopyridine/2-hydroxyterephthalic acid composite salt (TH salt)  2  3  5  6-tetraaminopyridine hydrochloride(TAPH)  2-hydroxyterephthalic acid(HTA)  3  5- dinitropyridine-2  6-diamine(DADNP)  
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