草铵膦关键中间体氯代亚磷酸二乙酯合成工艺研究
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摘要
氯代亚磷酸二乙酯作为格氏法合成草铵膦关键中间体,其下游产物甲基亚磷酸二乙酯是重要的有机化工中间体,广泛应用于农药、医药等行业。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,实验考查并优化了原料配比、反应温度、保温时间等一系列条件,所得氯代亚磷酸二乙酯质量分数为94.5%,收率达94.5%。
Diethyl chlorophosphite is the key intermediate of glufosinate synthesis by Grignard method. Its downstream product diethyl phosphite is an important organic chemical intermediate widely used in pesticides, pharmaceuticals and other industries. In this paper, a series of conditions, such as the raw material ratio, reaction temperature, holding time and so on,were experimentally investigated and optimized by using phosphorus trichloride as the starting material and the disproportionation reaction to synthesize diethyl chlorophosphite. Diethyl phosphate mass fraction of 94.5%, 94.5% yield.
Diethyl chlorophosphite is the key intermediate of glufosinate synthesis by Grignard method. Its downstream product diethyl phosphite is an important organic chemical intermediate widely used in pesticides, pharmaceuticals and other industries. In this paper, a series of conditions, such as the raw material ratio, reaction temperature, holding time and so on,were experimentally investigated and optimized by using phosphorus trichloride as the starting material and the disproportionation reaction to synthesize diethyl chlorophosphite. Diethyl phosphate mass fraction of 94.5%, 94.5% yield.
引文
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[3]蒋红英,刘书来,张建友,等.有机磷和菊酯类农药在蔬菜中的氧化消降技术研究[J].浙江工业大学学报, 2010, 38(4):368-371.
[4]联邦德国Hoechst公司农业开发部.草丁膦[J].农药译丛,1985,7(1):62-64.