核磁共振磷谱在羟基亚乙基二磷酸合成中的应用
收稿日期: 2014-05-19
修回日期: 2015-01-11
网络出版日期: 2015-03-05
Synthesis of 1-Hydroxyethylidene-1,1-Diphosphonic Acid (HEDP) Monitored by 31P NMR
Received date: 2014-05-19
Revised date: 2015-01-11
Online published: 2015-03-05
讨论了羟基亚乙基二磷酸的反应机理，并通过核磁共振磷谱对合成反应过程中的中间体亚磷酸和关键中间体(3)的实时监测．在此基础上优化了反应条件．最后，对原料三氯化磷中的杂质进行合理分析和排除．
关键词： 核磁共振磷谱(31P NMR); 羟基亚乙基二磷酸; 工艺优化
施波 , 杜成堂* , 庄东青 . 核磁共振磷谱在羟基亚乙基二磷酸合成中的应用[J]. 波谱学杂志, 2015 , 32(1) : 116 -122 . DOI: 10.11938/cjmr20150113
In this paper, we report the use of 31P NMR to monitor the synthesis process of 1-hydroxyethylidene-1,1-diphosphonic acid (HEDP). 31P NMR was used to detect signals from the residues of key intermediates phosphorous acid and 3. The synthesis process was optimized based on the 31P NMR results. Impurity such as PCl3 were analyzed.
Key words： 31P NMR; HEDP; process optimization
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