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Synthesis method of ethyl methyl-(3-oxo-propyl)phosphinate

A synthesis method and technology of phosphonaldehyde, which is applied in the field of synthesis of phosphonaldehyde, can solve the problems of low yield, safety and occupational injury, and achieve the effects of improving reaction efficiency, simple and easy control of the operation process, and increasing the yield of phosphonaldehyde

Inactive Publication Date: 2017-10-10
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are many foreign literatures reporting the preparation method of phosphonaldehyde, for example: Meiji Seika patent acrolein first generates acetal with ethanol and then reacts with diethyl methyl phosphite to prepare phosphonaldehyde, but the yield is low; Hoechst patent Using acetic anhydride acrolein and diethyl methyl phosphite as raw materials, acetic anhydride and acrolein first react to form diacetyl propylene, then add diethyl methyl phosphite, and then remove the acetyl group to obtain phosphonic aldehyde. It has a high yield, but there are problems of safety and occupational injury caused by ether in the product

Method used

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Examples

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Effect test

Embodiment 1

[0024] A method for synthesizing phosphonic aldehydes. The phosphonic aldehydes are prepared by using absolute ethanol as a solvent, glacial acetic acid, acrolein and diethyl methylphosphite as raw materials, mixing and reflux reaction.

[0025] The phosphonic aldehyde obtained by the method can be directly used in the glufosinate-ammonium synthesis process, or the obtained phosphonic aldehyde can be sent to the glufosinate-ammonium synthesis process after distillation to remove ethanol and ethyl acetate in the reaction process.

Embodiment 2

[0027] This embodiment is a further description of the mixing process in Example 1. The specific operation of mixing can be: use absolute ethanol as a solvent to prepare diethyl methylphosphite ethanol liquid, acetic acid ethanol liquid and acrolein ethanol liquid respectively , Add diethyl methylphosphite ethanol solution and acetate ethanol solution dropwise to acrolein ethanol solution at the same time.

[0028] During the mixing process, the molar ratio of glacial acetic acid, absolute ethanol and diethyl methyl phosphite was controlled at 1:40:1.

Embodiment 3

[0030] The difference between this embodiment and embodiment 2 is that the specific operations of mixing are different. In this embodiment, the mixing steps include:

[0031] A: Add absolute ethanol and glacial acetic acid into the container, then add diethyl methyl phosphite, stir well and get a mixed solution, set aside;

[0032] B: Add absolute ethanol and acrolein into another container, stir evenly, and add the mixed solution prepared in step A dropwise during the stirring process.

[0033] During the mixing process, the molar ratio of glacial acetic acid, absolute ethanol and diethyl methyl phosphite was controlled at 1.5: 3: 1.

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Abstract

The invention discloses a synthesis method of phosphonic aldehyde. The phosphonic aldehyde is prepared by using absolute ethanol as a solvent, glacial acetic acid, acrolein and diethyl methylphosphite as raw materials, mixing, heating and distillation. The yield of this method is significantly higher than that of the Japanese Meiji Seika patent, up to 93.3%, which is close to the product yield of the Hoechst patent, and at the same time avoids the safety and occupational injuries caused by the generation of ether, meets the requirements of clean production, and has good practicality. sex.

Description

technical field [0001] The present invention is a synthesis method of phosphine aldehyde, specifically relates to the synthesis method of methyl-(3-oxo-propyl) ethyl phosphinate (referred to as "phosphine aldehyde"), which is an intermediate product of glufosinate ammonium, and belongs to organic phosphine chemistry. The field of synthetic technology. Background technique [0002] Phosphonic aldehyde is an intermediate for the synthesis of organophosphorus compounds and an important intermediate for the herbicide glufosinate. Glufosinate-ammonium is an ideal herbicide for transgenic resistant crops, with the characteristics of high efficiency, low toxicity and broad herbicidal spectrum. With the rapid development of genetically modified crops, such as genetically modified glufosinate-resistant rice and genetically modified glufosinate-resistant soybeans, the market demand for glufosinate is also increasing rapidly. The chemical properties of phosphonaldehyde are lively, it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32
CPCC07F9/3211
Inventor 张华姜永红任成湘阮冬冬
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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