High yield synthetic method for quizalofop-p-ethyl

A synthetic method, the technology of quizalofop-p-ethyl, which is applied in the field of pesticide product synthesis, can solve the problems of large solvent loss, high production cost, and long production cycle, and achieve the effects of less side reactions, short process, and reduced equipment costs

Inactive Publication Date: 2011-11-23
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problems of complex operation, large solvent loss, high production cost, long production cycle and low yield in the current industrialized production process, and provides a synthesis method using a single organic solvent and directly cooling and crystallizing without removing the solvent , so as to shorten the production process cycle, simplify the production process, improve the synthesis yield and reduce the production cost

Method used

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  • High yield synthetic method for quizalofop-p-ethyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 275kg of 6-chloro-2-(4-hydroxyphenoxy)quinoxaline with a content of 97.4% in a 5000L reactor with a water separation device, and pay attention to prevent static electricity with anti-static clips, and then put in sodium carbonate 250kg, open the solvent pipeline valve and inject 2750kg cyclohexane to close the manhole. In the metering tank, 298 kg of R (-) ethyl p-toluenesulfonyl lactate with a vacuum extraction content of 96% was used for subsequent use.

[0026] After the crank is flexible, start stirring, heat up and reflux to carry water until no more water droplets sink in the water separator, continue to carry water for 0.5 hours, and the reaction system is in an anhydrous state.

[0027] After the addition of water, keep the system in the state of reflux with water, and add R(-) ethyl p-toluenesulfonyl lactate dropwise at a uniform speed, which takes 4.5 hours. After the addition is completed, continue to react for 6 hours, and take samples for tracking.

[...

Embodiment 2

[0034] Put 400kg of 6-chloro-2-(4-hydroxyphenoxy)quinoxaline with a content of 97% in the 5000L reactor, pay attention to prevent static electricity with anti-static clips, then put in 230kg of potassium hydroxide, and open the solvent pipeline The valve measures 2400kg cyclohexanone as the reaction solvent, and the manhole is closed. In the metering tank, 423 kg of R (-) ethyl p-toluenesulfonyl lactate with a vacuum extraction content of 96.3% was used for subsequent use.

[0035] After the crank is flexible, start stirring, heat up and return to bring water until the water separator no longer sinks, continue to carry water for 0.5 hours, and the reaction system is in an anhydrous state. After carrying water, keep the system in the state of reflux with water, and add R(-) ethyl p-toluenesulfonyl lactate dropwise at a uniform speed, which takes 2 hours, and take samples for tracking after 10 hours of reaction. With gas chromatography analysis, 6-chloro-2-(4-hydroxyphenoxy gro...

Embodiment 3

[0040] Put 275kg of 6-chloro-2-(4-hydroxyphenoxy)quinoxaline with a content of 96.5% into the 5000L reactor, pay attention to prevent static electricity with anti-static clips, then put in 163kg of potassium hydroxide, and open the solvent pipeline Inject 2500kg cycloheptane into the valve to close the manhole. In the metering tank, 310 kg of R (-) ethyl p-toluenesulfonyl lactate with a vacuum extraction content of 95.8% was used for subsequent use.

[0041]After the crank is flexible, start stirring, heat up and return to bring water until the water separator no longer sinks, continue to carry water for 0.5 hours, and the reaction system is in an anhydrous state. After the addition of water, keep the system in the state of reflux with water and add R(-) ethyl p-toluenesulfonyl lactate dropwise at a constant speed for 4 hours. After the dropwise addition, continue to react for 4 hours to take samples for tracking. Analyze the content of 6-chloro-2-(4-hydroxyphenoxy)quinoxalin...

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Abstract

The invention relates to a synthetic method for quizalofop-p-ethyl, a high efficiency herbicide. The method comprises the four steps of water straining, substitution, rinsing and crystallization. According to the method, 6-chlorine-2-(4-hydroxyphenoxy)quinoxaline reacts with R(-)p-toluenesulfonyl ethyl lactate, alkali metal and salts thereof are employed as acid binding agents, a single organic solvent is employed as a reaction system, and solid-liquid separation is used for separating a product; the yield of the product exceeds 90%, the content of the product is about 97.5%, and the content of the active substance R is more than 94%. Compared to the conventional technology, the preparation method provided in the invention has the characteristics of little side reaction, a short flow, a stationary process, high yield of the product, high content of the active substance and low energy consumption.

Description

technical field [0001] The invention belongs to the technical field of pesticide product synthesis, and relates to a method for synthesizing quizalofop-p-ethyl, a herbicide in paddy fields. Background technique [0002] Quizalofop-ethyl is mainly used to control annual and perennial grass weeds in broad-leaved crops, such as barnyardgrass, foxtail, wild oats, brome, and stephae, and is ineffective against broad-leaved weeds. The product is a selective systemic conduction herbicide for stem and leaf treatment. The medicine is absorbed through the stems and leaves of the weeds, and is bidirectionally transmitted upwards and downwards. For annual grass weeds, the drug can spread throughout the whole plant within 24 hours, inhibit the synthesis of cells and fatty acids, and die. It has the characteristics of wide range of use and high efficiency [0003] At present, the main method for synthesizing quizalofop-p-p in China is to react in petroleum ether. After the reaction, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/44
Inventor 綦非栾波张建林刘英贤曹帅高洪奎
Owner JINGBO AGROCHEM TECH CO LTD
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