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作 者:梁吉连[1] 吴广文[1] 周耀华[1] 解世伟[1] 龚小红[1]
机构地区:[1]武汉工程大学化工与制药学院湖北省新型反应器与绿色化学工艺重点实验室,湖北武汉430074
出 处:《武汉工程大学学报》2011年第11期23-26,共4页Journal of Wuhan Institute of Technology
摘 要:氨基胍溶液和草酸经酰化、环合生成3-氨基三氮唑-5-羧酸,总收率为76.8%,纯度95.67%.考察了原料配比,母液套用,反应温度和水用量等因素对反应的影响.结果表明:配料比为n(草酸)n(氨基胍)=1.31,母液套用2次时酰化产率较高;在60℃时1h滴加完硫酸,m(酰化物)m(水用量)=15时产品纯度与收率较佳.采用核磁共振氢谱,红外图谱和质谱对产物的结构进行了表征.3-Amino-triazole-5-carboxylic acid was proposed by acylating and cyclizating in condition of aminoguanidine and oxalic acid.Factors were investigated including the material ratio,mother liquor,reaction temperature and water consumption.The yield and purity of 3-Amino-triazole-5-carboxylic acid were 76.8% and 95.67% respectively under the optimal conditions:n(oxalicacid)n(aminoguanidine)=1.31,mother liquor was applied twice,sulfuric acid was completed dropping 1 h at 60 ℃ and m(acylation)m(water consumption)=15.The synthetic compounds were characterized by IR,1H NMR and mass spectra.
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