A kind of synthetic method of glufosinate ammonium salt

Abstract

The invention relates to a synthesizing method for glufosinate-ammonium ammonium salt. The synthesizing method comprises the following steps: 1) synthesizing methyl methoxyphosphoryl propionate by the reaction of methyl phosphite dimethyl phosphate with methyl acrylate and methyl alcohol; 2) synthesizing 2-[(methyl methoxy)phosphoryl]methyl-3-oxo-butyrate dimethyl ester by the Claisen condensation of methyl methoxyphosphoryl propionate and dimethyl oxalate; 3) under the acidic condition, carrying out the hydrolysis reaction to the 2-[(methyl methoxy)phosphoryl]methyl-3-oxo-butyrate dimethyl ester so as to generate 4-hydroxymethylphosphonic oxide butyric acid; and 4) under the catalyst function, successively reacting with ammonia gas and hydrogen by the 4-hydroxymethylphosphonic oxide butyric acid, and preparing the glufosinate-ammonium ammonium salt. The synthesizing method is capable of avoiding using cyanide poisonous materials. The format reaction is not used, the amount of the solvent used in the production process is small, the reaction condition is moderate and easily controlled, the synthesizing method is suitable for industrial production, the production is safe and convenient to operate, the reaction process is short, and the yield is high.

Description

technical field [0001] The invention belongs to a preparation method of glufosinate-ammonium, in particular to a synthesis method of glufosinate-ammonium salt. Background technique [0002] Glufosinate-ammonium is a highly efficient, low-toxic, non-selective (killing) contact organic phosphine herbicide with partial systemic action, which was first developed by the German company Hoechst. Its synthesis methods include fermentation and chemical synthesis. The fermentation method is mainly to produce bialaphos by microbial fermentation. Most of the chemical synthesis methods use phosphine trichloride or phosphite as the starting material and react with certain amino derivatives. [0003] At present, the synthesis methods of glufosinate-ammonium mainly include high-pressure catalytic synthesis method, low-temperature directional synthesis method, Gabriel-diethyl malonate synthesis method, Abzov-Michael method and Stryker-Zelinsky method. etc., but all there are various probl...

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Problems solved by technology

[0003] At present, the synthesis methods of glufosinate-ammonium mainly include high-pressure catalytic synthesis method, low-temperature directional synthesis method, Gabriel-diethyl malonate synthesis method, Abzov-Michael method and Stryker-Zelinsky method. etc., but all there are various problems in it, such as using carbon monoxide and hydrogen in the high-pressure catalytic synthesis method, and reacting under a high pressure of 15-20MPa, the requirements for equipment are high, and it is not suitable for industrial production. In addition, carbon monoxide is also a highly toxic gas, which is not very Good control; the anionization process of hydrogenated pyrazine in the low-temperature directional synthesis method requires a low temperature of -80°C, which is not easy for industrial production; in addition, the n-butyllithium used is also an extremely dangerous flammable and explosive product, and accidents are likely to occur if improper operation is performed; The Gabriel-diethyl malonate synthesis method requires the use of chlorine and bromine, which is difficult to control during industrialization and has high costs; the Abzov-Michael method was proposed by a postgraduate student at the School of Materials Science and Technology, Southwest University of Science and Technology, but its Grignard reagents are used, which are difficult to control during industrialization; the Stryker-Zelinsky method is disclosed by the patent of the preparation method (patent No. 98808261) applied by Germany Hearst-Schering Agricultural Development Co., Ltd. in August 1998 , the reaction is to prepare glufosinate-ammonium by reacting diethyl methylphosphinate with acrolein under conditions such as acid anhydride, and then reacting with cyanide to prepare glufosinate-ammonium. In the reaction, highly toxic potassium cyanide or sodium is used, which is easy to cause pollution and personal injury; and a large amount of organic solvents such as alcohol, ether, tetrahydrofuran are needed in the reaction, and the cost is high

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