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Method for synthesizing herbicide fenoxaprop-p-ethyl

A technology for oxaflufen-ethyl and dichlorobenzoxazole is applied in the field of synthesizing the herbicide oxaflufen-ethyl, which can solve problems such as insufficient synthesis methods, difficult wastewater treatment, and achieve simple treatment and production cost savings. Effect

Active Publication Date: 2020-10-02
JIANGSU FUDING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional synthetic reaction process of fenoxaprop-ethyl is a solid-liquid phase reaction, and the synthesis method has serious shortcomings, and a large amount of organic solvents are used in the production process, resulting in a large amount of nitrogen-containing wastewater, which is difficult to treat in the later stage
At present, there is also a liquid phase reaction to prepare fenoxaprop-ethyl, but there are large-scale separation of organic solvents or mixed solvents in the production process

Method used

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  • Method for synthesizing herbicide fenoxaprop-p-ethyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 48.4g of acetone and 19.4g of 2,6-dichlorobenzoxazole into a 250ml three-necked flask, stir at a temperature of 20-25°C, and dissolve.

[0023] Add 29.5g of water, 21g of R-(+)-2-(4-hydroxyphenoxy) ethyl propionate, 31.8g of sodium carbonate, 0.5g of benzyltriethylammonium chloride into a 250ml three-necked flask, stir, and heat up to 60°C and keep warm for 3 hours to obtain a mixed solution. Raise the temperature to 70°C, add the 2,6-dichlorobenzoxazole acetone solution dropwise to the mixture in the three-necked flask, the dropwise addition is completed in about 1 hour, after the dropwise addition is completed, keep the reaction at 70-75°C for 2 hours, add dropwise and keep warm During the reaction process, the acetone in the system was distilled off, and the acetone aqueous solution was collected.

[0024] After the reaction, keep the temperature of the system at 70-75°C, let stand for 30 minutes to separate the layers, separate the organic phase, add 30g of wat...

Embodiment 2

[0026] Add 48.4g of acetone and 19.4g of 2,6-dichlorobenzoxazole into a 250ml three-necked flask, stir at a temperature of 20-25°C, and dissolve.

[0027] Add 29.5g water, 21g R-(+)-2-(4-hydroxyphenoxy) ethyl propionate, 26.5g sodium carbonate, 0.5g benzyltriethylammonium chloride into a 250ml three-necked flask, stir, and heat up to 60°C and keep warm for 3 hours to obtain a mixed solution. Raise the temperature to 70°C, add the 2,6-dichlorobenzoxazole acetone solution dropwise to the mixture in the three-necked flask, the dropwise addition is completed in about 1 hour, after the dropwise addition is completed, keep the reaction at 70-75°C for 2 hours, add dropwise and keep warm During the reaction process, the acetone in the system was distilled off, and the acetone aqueous solution was collected.

[0028] After the reaction, keep the temperature of the system at 70-75°C, let it stand for 30 minutes to separate the layers, separate the organic phase, add 30g of water to the...

Embodiment 3

[0030] Add 48.4g of acetone and 19.0g of 2,6-dichlorobenzoxazole into a 250ml three-necked flask, stir at a temperature of 20-25°C, and dissolve.

[0031] Add 29.5g of water, 21g of R-(+)-2-(4-hydroxyphenoxy) ethyl propionate, 31.8g of sodium carbonate, 0.5g of benzyltriethylammonium chloride into a 250ml three-necked flask, stir, and heat up to 60°C and keep warm for 3 hours to obtain a mixed solution. Raise the temperature to 70°C, add the 2,6-dichlorobenzoxazole acetone solution dropwise to the mixture in the three-necked flask, the dropwise addition is completed in about 1 hour, after the dropwise addition is completed, keep the reaction at 70-75°C for 2 hours, add dropwise and keep warm During the reaction process, the acetone in the system was distilled off, and the acetone aqueous solution was collected.

[0032] After the reaction, keep the temperature of the system at 70-75°C, let stand for 30min to separate the layers, separate the organic phase, add 30g of water to...

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Abstract

The invention discloses a method for synthesizing fenoxaprop-p-ethyl, which comprises the following steps: dissolving 2,6-dichlorobenzoxazole in acetone at the temperature of 20-25 DEG C; mixing ethylR-(+)-2-(4-hydroxyphenoxy) propionate, inorganic base, a catalyst and water, and stirring at 60-65 DEG C to obtain a mixed solution; heating to 70-75 DEG C, dropwise adding the 2,6-dichlorobenzoxazole acetone solution into the mixed solution, after dropwise adding is completed, carrying out heat preservation reaction at 70-75 DEG C, evaporating out acetone in the reaction process, and collectingan acetone aqueous solution; standing and layering the reaction solution, adding water to wash an organic phase at 70-75 DEG C, then removing water to obtain a fenoxaprop-p-ethyl crude product, and recrystallizing with ethanol to obtain a fenoxaprop-p-ethyl product. According to the fenoxaprop-p-ethyl product disclosed by the invention, the content of effective optical rotation bodies in the fenoxaprop-p-ethyl product is 99.9% or above. Acetone is distilled off at atmospheric pressure in the reaction process, and high-purity recovery of the distilled acetone aqueous solution can be realized byadopting a membrane separation technology.

Description

technical field [0001] The invention belongs to the field of pesticide weeding, and in particular relates to a method for synthesizing the herbicide fenoxaprop-ethyl. Background technique [0002] Fenoxaprop-ethyl, chemically named (R)-2-[4-(6-chloro-2-benzoxazolyloxy)phenoxy]ethyl propionate, is a new type of hetero Ring herbicide, with high efficiency, low toxicity, and less environmental pollution; Fenoxaprop-ethyl is effective in preventing and controlling gramineous weeds in crops such as wheat and rye, such as acorns, wild oats, and foxtails. Very good control effect. The traditional process of synthesis of fenoxaprop-ethyl is a solid-liquid phase reaction, and the synthesis method has serious shortcomings. In addition, a large amount of organic solvents are used in the production process, resulting in a large amount of nitrogen-containing wastewater, which is difficult to treat in the later stage. At present, there is also the preparation of fenoxaprop-ethyl by liqu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D263/58
CPCC07D263/58
Inventor 刘东卫张彦飞
Owner JIANGSU FUDING CHEM
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