Synthesis method of glufosinate intermediate of methyl diethyl phosphite

Abstract

The invention discloses a synthesis method of glufosinate intermediate of methyl diethyl phosphate. According to the synthesis method, MDP is used as raw materials to take a reaction with an ethyl alcohol gas phase in a tubular reactor to generate methyl diethyl phosphate. The process operation process is simplified; the connection is ordered; the labor cost is greatly reduced; the production cost is reduced. The tubular reactor is used; the reaction equipment using a reaction kettle in the prior art is changed; the tubular reactor can realize the fast separation of a byproduct of hydrogen chloride from the product; the product yield is improved; meanwhile, the continuous operation is also realized; the danger in the industrialization process is avoided; the potential safety hazards are eliminated.

Description

technical field [0001] The invention relates to a synthesis method of an organophosphorus compound, in particular to a synthesis method of a herbicide glufosinate-ammonium intermediate, diethyl methyl phosphite. Background technique [0002] Glufosinate-ammonium is a phosphoric acid herbicide, which is currently the world's largest tonnage pesticide variety and the world's second largest genetically modified crop resistant to herbicides, and diethyl methyl phosphite is an important synthesis of glufosinate-ammonium intermediate, so the synthesis of diethyl methylphosphite is crucial. [0003] At present, it has been reported in the literature that the route for the synthesis of glufosinate-ammonium using diethyl methyl phosphite as an intermediate: Hans-Joachim Zeiss once reported using methyl phosphite in J.Org.Chem.1991,56,1783-1788 Diethyl phosphate and ethyl acrylate are catalyzed under alkaline conditions to produce diethyl methyl phosphite with a yield of 81%, and the...

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Problems solved by technology

[0004] The synthesis of diethyl methyl phosphite in China is still in the small test stage. For example, the Chinese invention patent (ZL201310299754.7) discloses a synthesis method of diethyl methyl phosphite, which includes the following steps: diethyl phosphite Ester and methyl chloride gas are reacted in the presence of an acid-binding agent to prepare diethyl methylphosphonate, filtered after the reaction, and the diethyl methylphosphonate generated exists in the filtrate; Organic solvent solution, reducing diethyl methylphosphonate to diethyl methylphosphonite, distilling the reaction solution after the reaction to obtain diethyl methylphosphonite, the synthesis method uses a reactor, and the reaction requirements are high , and needs to be carried out under solvent conditions, subsequent distillation and other processes are required, which consumes a lot of energy, which is not conducive to energy saving and emission reduction; in addition, there are reports that MDP is added dropwise to ethanol using a reactor, and triethylamine or pyridine or ammonia is used as a bond. Acid agent, due to the limitation of the structure of the reactor, the reaction needs to be carried out under solvent conditions. In addition, due to the instability of MDP, it is easy to react with the added alkaline substances under suitable conditions. On the one hand, the loss of raw materials is large, and the cost of raw materials increases sharply. On the other hand, the yield of the product is low, which affects the production of the product, and then affects the normal production of the company

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