摘要
以乙醇胺和3-氨甲基吡啶为原料分别与甲醛和亚磷酸通过Manich反应合成了乙醇胺二甲叉磷酸和3-氨甲基吡啶二甲叉磷酸,并对乙醇胺二甲叉磷酸的合成条件进行了探讨研究,最终确定了其最佳合成条件:当乙醇胺:亚磷酸:甲醛=1∶2∶3.5(摩尔比),反应温度为100℃,回流时间为3 h时,产品的收率(以乙醇胺计)为77.3%,以同样方法合成的3-氨甲基吡啶二甲叉磷酸的收率(以3-氨甲基吡啶计)为80.1%.产物通过红外光谱、^(31)P-NMR谱、~1H-NMR谱和元素分析方法进行了表征.
Ethanolamine dimethylenephosphonic acid and P,P’-[[(3-pyridinyl-methyl)imino]bis(methylene)]bis-phosphonic acid were synthesized by Manich reaction with ethanolamine and 3-pyridinemethanamine as raw materials,respectively. The optimum synthesis conditions for ethanolamine dimethylenephosphonic acid were as follows:the mole ratio of ethanolamine,phosphorous acid and formaldehyde was 1∶ 2∶ 3.5,the reaction temperature was 100 ℃,and the reaction time was 3.5 h. The yield was about 77.3%(based on ethanolamine).P,P’-[[(3-pyridinylmethyl)imino]bis(methylene)]bis-phosphonic acid was obtained by the same method and the yield was about 80.1%(based on 3-pyridinemethanamine). The products were characterized by infrared spectroscopy,31P-NMR and 1H-NMR spectroscopy and elemental analysis.
出处
《武汉工程大学学报》
CAS
2016年第2期114-119,共6页
Journal of Wuhan Institute of Technology
关键词
Manich反应
乙醇胺二甲叉磷酸
3-氨甲基吡啶二甲叉磷酸
manich reaction
ehtanolamine dimethylenephosphonic acid
P,P’-[[(3-pyridinylmethyl)imino] bis(methylene)]bis-phosphonic acid