甲基亚磷酸二乙酯合成工艺研究  

Research on the synthetic process of diethyl methyl-phosphonite

作　　者：丁成荣[1] 郭伟晨 梁鸿飞[1] 季方良 张国富[1] 杨华东[1] 

机构地区：[1]浙江工业大学化学工程学院,浙江杭州310014

出　　处：《浙江工业大学学报》2016年第2期150-153,共4页Journal of Zhejiang University of Technology

基　　金：国家自然科学基金资助项目(20702051);浙江省自然科学基金资助项目(LY13B020017);浙江省科技重点创新团队(2010R50018)

摘　　要：甲基亚磷酸二乙酯是农药、医药的关键有机化工中间体,为了降低与其相关产品的生产成本,设计了以三氯化磷为起始原料,经歧化反应合成中间体氯代亚磷酸二乙酯,再经甲基化反应合成甲基亚磷酸二乙酯.通过对反应物料摩尔比、反应温度及催化剂的种类进行优化,所得产品纯度达97.6%,反应总收率达78.5%,产物结构经1 HNMR,GC-MS,IR进行表征确认.该工艺采用独创的复合型催化剂,有效的抑制了副反应,提高主产物的纯度及收率,具有较好的工业化应用前景.Diethyl methyl-phosphonite is a key intermediate in organic chemical industry.In order to diminish the cost of production of its relevant products,we determine using phosphorus trichloride and triethyl phosinite to give diethyl phosphonate chloride,then reacting with Grignard reagent to produce diethyl methyl-phosphonite.The effects of material ratio,reaction temperature and the catalyst types on the yield were studied.This synthetic approache could give an excellent total yield of 78.5% under a higher purity of 97.6%.Its structure was characterized by 1 HNMR,GC-MS and IR.A newly developed complex catalyst was employed.It can restrain the formation of by-products effectively and then increase the purity and the yield of the main product.It has great potential in industrial applications.

关 键 词：中间体 甲基亚膦酸二乙酯 合成 

分 类 号：TQ460.3[化学工程—制药化工]