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| -5-巯基-1H-四氮唑的制备 | |
| 引用本文： | 李永伟,王 娟,李瑞民,朱智甲,白文举.-5-巯基-1H-四氮唑的制备[J].河北工业科技,2015,32(1):8-11. |
| 作者姓名： | 李永伟 王 娟 李瑞民 朱智甲 白文举 |
| 作者单位： | 1. 河北常山生化药业股份有限公司,河北石家庄,050800 2. 石家庄学院化工学院,河北石家庄,050035 3. 东华大学化学化工与生物工程学院,上海,201620 |
| 摘 要： | 介绍了一种1-2-(N,N-二甲基氨基)乙基]-5-巯基-1H-四氮唑(DMMT)的合成方法。2-(N,N-二甲基氨基)乙胺与二硫化碳反应,制得取代的2-(N,N-二甲基氨基)乙胺基二硫代羧酸;2-(N,N-二甲基氨基)乙胺基二硫代羧酸与氯甲酸乙酯反应,得到2-(N,N-二甲基氨基)乙胺基二硫代羧酸与乙氧基甲酸的二硫代酸酐;二硫代酸酐再经三乙胺碱解,制得2-(N,N-二甲基氨基)乙基异硫氰酸酯;2-(N,N-二甲基氨基)乙基异硫氰酸酯与叠氮化钠反应,制得目标产物1-2-(N,N-二甲基氨基)乙基]-5-巯基-1H-四氮唑(DMMT)。产物以N,N-二甲基氨基乙胺计,收率为48.0%。采用该法,能够方便地制得1-2-(N,N-二甲基氨基)乙基]-5-巯基-1H-四氮唑,产物收率高,反应条件温和,操作过程简便,三废少,环境污染小。 |
| 关 键 词： | 有机合成化学 1-[2-(N N-二甲基氨基)乙基]-5-巯基-1H-四氮唑 氯甲酸乙酯 叠氮化钠 合成 |
| 收稿时间： | 2014/8/18 0:00:00 |
| 修稿时间： | 2014/9/23 0:00:00 |
Preparation of 1-(2-(N,N-dimethylamino)ethyl)-5-thio-1H-tetrazole |
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| LI Yongwei,WANG Juan,LI Ruimin,ZHU Zhijia and BAI Wenju.Preparation of 1-(2-(N,N-dimethylamino)ethyl)-5-thio-1H-tetrazole[J].Hebei Journal of Industrial Science & Technology,2015,32(1):8-11. | |
| Authors: | LI Yongwei WANG Juan LI Ruimin ZHU Zhijia and BAI Wenju |
| Institution: | LI Yongwei;WANG Juan;LI Ruimin;ZHU Zhijia;BAI Wenju;Hebei Changshan Biochemical Pharmaceutical Company Limited;School of Chemical Engineering,Shijiazhuang University;College of Chemistry,Chemical Engineering and Biotechnology,Donghua University; |
| Abstract: | A synthetic method of DMMT is introduced. 2-(N,N-dimethylamine) ethylamine reacts with carbon disulfide and it gives substitutional 2-(N,N-dimethylamino) ethylamincarbodithioic acid. The substitutional acid reacts with ethyl chloroformate and it gives disulfide generation anhydride of 2-(N,N-dimethylamino) ethylamincarbodithioic acid and ethyoxyl methanoic acid. Then through triethylamine alkaline hydrolysis, 2-(N,N-dimethyl amine) ethyl isothiocyanate is obtained, and it reacts with NaN3 to give the desired product with 48% overall yield (counted with N,N-dimethyl amino ethyl amine). This procesure can prepare DMMT conveniently, and has the characteristics of high yield, mild process, simple operation, less waste and less pollution. |
| Keywords: | organic synthesis chemistry 1-[2-(N N-dimethylamino) ethyl]-5-thio-1H-tetraiazole(DMMT) ethyl chloroformate NaN3 synthesis |
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