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

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

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。

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%.