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Preparation method of methyl propanal ethyl phosphonate as glufosinate-ammonium intermediate

A technology of ethyl methylpropionyl phosphonate and ethyl methylpropionyl phosphonate, which is applied in the field of preparation of ethyl methylpropionyl phosphonate, an intermediate of glufosinate-ammonium, and can solve the problem of unzipping process The process is cumbersome, the yield is not very ideal, and it is not easy to recycle, etc., to achieve the effect of wide weeding spectrum, not easy to drift, safe and convenient to use

Active Publication Date: 2017-10-24
内蒙古佳瑞米精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deshrinking process of this route is cumbersome, the yield is not very ideal, the excess acid is not easy to recycle, and it will corrode the equipment.
This restricts the application of this method in industrialization
[0004] And in the prior art, use 3,3-diethoxypropyl methylphosphonic acid ethyl ester as raw material to prepare the method for ethyl methylpropanal group phosphonate, adopt hydrochloric acid as catalyst, its existence yield is low, not easy Recycling and other issues

Method used

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  • Preparation method of methyl propanal ethyl phosphonate as glufosinate-ammonium intermediate
  • Preparation method of methyl propanal ethyl phosphonate as glufosinate-ammonium intermediate
  • Preparation method of methyl propanal ethyl phosphonate as glufosinate-ammonium intermediate

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Effect test

Embodiment 1

[0032] A preparation method of glufosinate-ammonium intermediate methyl propionyl phosphonate, said preparation method comprising the steps of:

[0033] ①Add 100g of ethyl 3,3-diethoxypropylmethylphosphonate (content: 95%, 0.4mol), 18g of water (1mol) and 3g of sulfonic acid resin into a 500mL four-necked bottle, and stir , heated to 30°C, the measured pH value was 1.5, and kept at constant temperature for 2h;

[0034] ②Filtrate the product obtained in step ① to remove the sulfonic acid resin, add the filtrate into a 250mL single-necked bottle, and remove the solvent under reduced pressure by rotary evaporation. Ethyl ester 67.8g, figure 1 and figure 2 Its H NMR spectrum and gas mass analysis chart respectively. After testing, the purity of ethyl methylpropionyl phosphonate was 98% (GC), and the yield was 98.2%.

Embodiment 2

[0036] A preparation method of glufosinate-ammonium intermediate methyl propionyl phosphonate, the difference from Example 1 is: the reaction temperature in step 1. is 50°C; obtain 67g of methyl propionyl phosphonate, It has a purity of 97% (GC) and a yield of 96.2%.

Embodiment 3

[0038] A preparation method of glufosinate-ammonium intermediate methyl propionyl phosphonate, the difference from Example 1 is: the precipitation temperature in step ② is 65°C; obtain ethyl methyl propionyl phosphonate 65.6 g, its purity is 96.2% (GC), and its yield is 95.7%.

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Abstract

The invention relates to a preparation method of methyl propanal ethyl phosphonate as a glufosinate-ammonium intermediate and belongs to the field of organic chemistry. The preparation method comprises the following steps: (1) taking 3,3-diethoxy propyl methyl ethyl phosphonate as a raw material, catalyzing and hydrolyzing via a catalyst to prepare methyl propanal ethyl phosphonate, wherein the catalyst is sulfonic acid resin, strong acid ion exchange resin or perfluorinated sulfonic acid resin; and (2) filtering the product obtained in the step (1) for recycling sulfonic acid resin, and carrying out pressure-reduced desolvation of filtrate to obtain methyl propanal ethyl phosphonate. The specific preparation method is as shown in the description. According to the preparation method of methyl propanal ethyl phosphonate as the glufosinate-ammonium intermediate, through optimization of the catalyst, the reaction time is greatly reduced; the yield is improved; meanwhile, the catalyst is easy to recycle and is reusable; the production cost is reduced.

Description

technical field [0001] The invention relates to a preparation method of ethyl methyl propionyl phosphonate, an intermediate of glufosinate-ammonium, and belongs to the field of organic chemistry. Background technique [0002] Glufosinate-ammonium (glufosinate-ammonium) is developed and produced by Hearst Company. It is a phosphonic acid herbicide, a glutamine synthesis inhibitor, and a non-selective (killing) contact herbicide. It was developed in the 1980s and registered as a herbicide in 1984. Glufosinate-ammonium is a large-tonnage pesticide variety in the world, and it is also the second largest genetically modified crop resistant to herbicides in the world. Low toxicity, relatively safe, easy to degrade in soil, safe for crops, not easy to drift, wide herbicidal spectrum, high activity, less dosage, less environmental pressure, rapid herbicide, can quickly kill more than 100 species of Gramineae and broadleaf For leaf weeds, water can be used as a base, and it is safe...

Claims

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Application Information

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IPC IPC(8): C07F9/32
CPCY02P20/584C07F9/3211C07F9/3264
Inventor 董永侠向彬李君
Owner 内蒙古佳瑞米精细化工有限公司
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