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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

杨健,金宁人,张青龙,张清义   

  1. 浙江工业大学化工与材料学院,浙江 杭州 310032
  • 出版日期:2014-06-05 发布日期:2014-06-05

Synthesis of 2,3,5,6-tetraaminopyridine and its 2-hydroxyterephthalic acid composite salt

YANG Jian,JIN Ningren,ZHANG Qinglong,ZHANG Qingyi   

  1. College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou 310032,Zhejiang,China
  • Online:2014-06-05 Published:2014-06-05

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

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%.

Key words: 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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