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[1]梁吉连,吴广文*,周耀华,等.3氨基三氮唑5羧酸的合成工艺[J].武汉工程大学学报,2011,(11):23-26.
 LIANG Ji lian,WU Guang wen,ZHOU Yao hua,et al.Synthesis technology of 3Aminotriazole5carboxylic acid[J].Journal of Wuhan Institute of Technology,2011,(11):23-26.
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2011年11期
页码:
23-26
栏目:
化学与化学工程
出版日期:
2011-11-30

文章信息/Info

Title:
Synthesis technology of 3Aminotriazole5carboxylic acid
文章编号:
16742869(2011)11002304
作者:
梁吉连吴广文*周耀华解世伟龚小红
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
Author(s):
LIANG JilianWU GuangwenZHOU Yao huaXIE ShiweiGONG Xiaohong
Hubei Key Laboratory of Novel Chemical Reactor and Green Chemical Technology,
School of Chemical Engineering and Pharmacy,Wuhan Institute of Technology,Wuhan 430074,China
关键词:
三氮唑酰化环合工艺
Keywords:
triazoleacylationcyclizationtechnology
分类号:
TQ463.5
DOI:
-
文献标志码:
AAdoi:10.3969/j.issn.16742869.2011.11.006
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)=1.31,母液套用2次时酰化产率较高;在60 ℃时1 h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.
Abstract:
 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.

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