两种二甲叉磷酸衍生物的合成

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3h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、31P-NMR谱、1H-NMR谱和元素分析方法进行了表征.

Synthesis of Dimethylene Phosphoric Acid Derivatives

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 rawmaterials，respectively. The optimum synthesis conditions for ethanolamine dimethylenephosphonic acid wereas follows:the mole ratio of ethanolamine，phosphorous acid and formaldehyde was 1∶ 2∶ 3.5，the reactiontemperature was 100 ℃，and the reaction time was 3.5h. The yield was about 77.3%（based on ethanolamine） .P，P’-［［（3-pyridinylmethyl）imino］bis（methylene）］bis-phosphonic acid was obtained by the same methodand the yield was about 80.1%（based on 3-pyridinemethanamine） . The products were characterized by infraredspectroscopy， 31P-NMR and 1H-NMR spectroscopy and elemental analysis.