(羟基苯基)磷酰基乙酸的合成研究  

Research on(Hydroxyphenyl) Phosphinyl Acetic Acid Synthesis

作　　者：孙伟民[1] 

机构地区：[1]辽宁石化职业技术学院石油化工系,锦州121001

出　　处：《精细石油化工进展》2012年第10期28-31,共4页Advances in Fine Petrochemicals

摘　　要：将苯基亚磷酸的磷羟基进行硅保护,在80℃下进行Arbuzov反应5 h,然后再去保护并酸化,得到最终产品(羟基苯基)磷酰基乙酸(HPA)。通过1H NMR对中间体和目标产物的结构进行了表征。考察了原料配比、Arbuzov反应的温度与时间等因素对合成中间体(羟基苯基磷酰基)乙酸叔丁酯(HPAB)反应的影响,研究了HPAB酸化为HPA并重结晶提纯的影响因素,优化了反应条件。在最佳反应条件下,产品的固体收率为50.56%,wHPA≥98.5%。（Hydroxyphenyl） phosphinyl acetic acid （HPA） product was synthesized in the following process, in which phosphorus hydroxyl of phenyl phosphorous acid was silicon - protected and then subjected to Arbuzov reaction at 80 ℃for 5 h, and was de - protected and acidified afterwards. The structures of the intermediate and the target product were characterized by means of 1H - NMR. The effects of the factors like materials ratio, temperature and time duration of Arbuzov reaction, etc. on the reaction of synthesizing the intermediate, i.e. （ hydroxyphenyl phosphorus hydroxyl） tert - butyl acetate （ HPAB）, were investigated, the factors affecting the acidification of HPAB to HPA and the re - crystallization and purification of HPA were studied, and the reaction conditions were optimized. The yield of solid product reaches 50.56% with WHPA ≥ 98.5% under optimum reaction conditions.

关 键 词：(羟基苯基)磷酰基乙酸硅保护Arbuzov反应 

分 类 号：TQ265.1[化学工程—有机化工]