CAJ | 학술논문

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。
위료제비고순도여고수솔적2,3,5,6-사안기필정/2-간기대분이갑산복합염（TH염），통과이2,6-이안기-3,5이초기필정（DADNP）위원료최화가경환원제득2,3,5,6-사안기필정염산염（TAPH）。반응재55～60℃적경기분위하，이갑순위용제，Pd/C위최화제제득순도99.4%적TAPH，수솔82.1%。제성적염산염재화2-간기대분이갑산（HTA）납염재담기분위적보호하합성2,3,5,6-사안기필정/2-간기대분이갑산복합염（TH 염）단체，결구경과13C-NMR、MS화FT-IR표정분석，결과표명시목적산물，순도체98%이상。
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%.