3-氨基三氮唑-5-羧酸的合成工艺

Synthesis technology of 3-Amino-triazole-5-carboxylic acid

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)=1.31,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)=15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）=1.31,mother liquor was applied twice,sulfuric acid was completed dropping 1 h at 60 ℃ and m（acylation）m（water consumption）=15.The synthetic compounds were characterized by IR,1H NMR and mass spectra.