Preparation method of amino-nitrile and intermediate for preparing glufosinate-ammonium

A technology of aminonitrile and alkyl, which is applied in the field of pesticide preparation, can solve the problems of low yield of glufosinate-ammonium, and achieve the effects of easy industrial production, low production cost and high yield

Active Publication Date: 2015-04-08
GUANGAN LIER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the invention of the present invention is: in the existing method, adopt acetal To solve the problem of lo...

Method used

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  • Preparation method of amino-nitrile and intermediate for preparing glufosinate-ammonium
  • Preparation method of amino-nitrile and intermediate for preparing glufosinate-ammonium
  • Preparation method of amino-nitrile and intermediate for preparing glufosinate-ammonium

Examples

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Embodiment 1

[0031] (1) Preparation of ethyl 3,3-diethoxypropylmethylphosphonate

[0032] Add 143.2 g (1 mol) of diethyl methylphosphite with a content of 95% and 400 mL of absolute ethanol to a 1 L reaction flask, and add 57.7 g (1.02 mol) of acrolein with a content of 99% at a temperature of 20° C. dropwise under nitrogen protection. After the reaction at room temperature for 2 hours, the solvent and excess acrolein were recovered by distillation. The residue in the bottle was 243.5g, which was ethyl 3,3-diethoxypropylmethylphosphonate, with a content of 95% and a yield of 97.2%. .

[0033] (2) Preparation of ethyl 3-ethoxy allyl methyl phosphonate

[0034] At room temperature and in an inert gas protection atmosphere, 121.4g (0.5mol) of ethyl 3,3-diethoxypropylmethylphosphonate with a content of 98% was added to a 1L reaction flask, then 350g of tetrahydrofuran was added, cooled to 0°C, quickly add 41.2g (0.525mol) acetyl chloride dropwise, after the drop, the reactant was stirred at ...

Embodiment 2

[0038] (1) Preparation of methyl 3,3-dimethoxypropylmethylphosphonate

[0039] Add 170.5 g (1.5 mol) of dimethyl methylphosphite with a content of 95% and 500 mL of anhydrous methanol into a 1 L reaction flask, and add 87.7 g (1.55 mol) of acrolein with a content of 99% at 25°C under nitrogen protection, After dripping, react at room temperature for 2 hours, then distill to recover the solvent and excess acrolein. The residue in the bottle is 303.3g which is methyl 3,3-dimethoxypropylmethylphosphonate, with a content of 95% and a yield of 98% %.

[0040] (2) Preparation of 3-methoxyallyl methylphosphonic acid methyl ester

[0041] At room temperature and in an inert gas protection atmosphere, 303.3g (1.47mol) of 95% 3,3-dimethoxypropyl methylphosphonic acid methyl ester was added to a 1L reaction flask, cooled to -10°C, Quickly add 117g (1.49mol) of acetyl chloride dropwise. After the drop is completed, the reactant is stirred at room temperature for 2 hours, and the methyl ...

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Abstract

The invention discloses a preparation method of amino-nitrile and an intermediate for preparing glufosinate-ammonium. The preparation method disclosed by the invention aims at solving the problem of low glufosinate-ammonium yield by using acetal in the existing methods. Different from the existing methods for preparing glufosinate-ammonium, the method disclosed by the invention comprises the following steps: firstly reacting acetal with acetylchloride to obtain an enol ether intermediate, reacting the enol ether intermediate with sodium cyanide to obtain amino-nitrile, and finally hydrolyzing the amino-nitrile to obtain the glufosinate-ammonium. The method has the advantages of higher reaction yield and capacity of remarkably reducing the production cost of the glufosinate-ammonium.

Description

technical field [0001] The invention relates to the field of pesticide preparation, especially a new method for chemically synthesizing glufosinate-ammonium, specifically a method for preparing aminonitrile and an intermediate used for preparing glufosinate-ammonium. The invention successfully synthesizes an enol ether highly active intermediate glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is an organophosphorus non-selective contact herbicide, which can be used in orchards, vineyards, non-cultivated land, potato fields, etc. to control annual and perennial dicotyledonous and grassy weeds, perennial grassy weeds and sedges, Has a good effect. In addition, with the promotion of genetically modified crops, the demand for glufosinate-ammonium is increasing worldwide. [0003] Acetal It is an important precursor for the synthesis of glufosinate-ammonium. Patent WO79 / 00405 and CN101418013 have reported the process of synthesizing glufosinate-ammon...

Claims

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Application Information

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IPC IPC(8): C07F9/32C07F9/30
Inventor 曾柏清程柯范谦
Owner GUANGAN LIER CHEM CO LTD
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