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A kind of method of synthesizing herbicide fenoxafen

A technology for oxaflufen-ethyl and dichlorobenzoxazole, which is applied in the field of synthesizing herbicide oxaflufen-ethyl, can solve problems such as insufficient synthesis method and difficult waste water treatment, and achieves simple treatment and production cost saving. Effect

Active Publication Date: 2022-08-05
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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  • A kind of method of synthesizing herbicide fenoxafen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0023] In a 250ml three-necked flask, add 29.5g of water, 21g of R-(+)-2-(4-hydroxyphenoxy)ethyl propionate, 31.8g of sodium carbonate, and 0.5g of benzyltriethylammonium chloride, stir, and heat up. to 60°C, and kept for 3h to obtain a mixed solution. The temperature was raised to 70°C, and the 2,6-dichlorobenzoxazole acetone solution was added dropwise to the mixture in the three-necked flask. The dropwise addition was completed for about 1 hour. During the reaction, the acetone in the system was evaporated, and the acetone aqueous solution was collected.

[0024] After the reaction is completed, keep the temperature of the system at 70-75°C, let stand for 30min to separate layers, separate the organic phase, add 30g of water to the organic phase, keep the temperature at 70-75°C, stir and wash for 30min, stand for 30min, separa...

Embodiment 2

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

[0027] In a 250ml three-necked flask, add 29.5g of water, 21g of R-(+)-2-(4-hydroxyphenoxy)ethyl propionate, 26.5g of sodium carbonate, 0.5g of benzyltriethylammonium chloride, stir, and heat up to 60°C, and kept for 3h to obtain a mixed solution. The temperature was raised to 70°C, and the 2,6-dichlorobenzoxazole acetone solution was added dropwise to the mixture in the three-necked flask. The dropwise addition was completed for about 1 hour. During the reaction, the acetone in the system was evaporated, and the acetone aqueous solution was collected.

[0028] After the reaction is completed, keep the temperature of the system at 70-75°C, let stand for 30min to separate layers, separate the organic phase, add 30 g of water to the organic phase, keep the temperature at 70-75°C, stir and wash for 30min, stand for 30min, and separa...

Embodiment 3

[0030] 48.4g of acetone and 19.0g of 2,6-dichlorobenzoxazole were added to a 250ml three-necked flask, stirred at a temperature of 20-25°C, and dissolved.

[0031] In a 250ml three-necked flask, add 29.5g of water, 21g of R-(+)-2-(4-hydroxyphenoxy)ethyl propionate, 31.8g of sodium carbonate, and 0.5g of benzyltriethylammonium chloride, stir, and heat up. to 60°C, and kept for 3h to obtain a mixed solution. The temperature was raised to 70°C, and the 2,6-dichlorobenzoxazole acetone solution was added dropwise to the mixture in the three-necked flask. The dropwise addition was completed for about 1 hour. During the reaction, the acetone in the system was evaporated, and the acetone aqueous solution was collected.

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

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Abstract

The invention discloses a method for synthesizing oxaflufen-ethyl, comprising: dissolving 2,6-dichlorobenzoxazole in acetone at a temperature of 20-25°C; dissolving R-(+)-2- (4-Hydroxyphenoxy) ethyl propionate, inorganic base, catalyst and water were mixed, and stirred at a temperature of 60-65 °C to obtain a mixed solution; the temperature was raised to 70-75 °C, 2,6-dichlorobenzoxane was mixed with The azole acetone solution is added dropwise to the mixed solution, after the dropwise addition is completed, the reaction is incubated at 70-75 °C, the acetone is evaporated during the reaction, and the acetone aqueous solution is collected; After dehydration, the crude oxaflufen-ethyl is obtained, which is recrystallized from ethanol to obtain the oxaflufen-ethyl product. The content of effective optically active bodies in the oxazolam product of the present invention is more than 99.9%. During the reaction process, acetone is distilled out at atmospheric pressure, and the distilled acetone aqueous solution can be recovered with high purity by means of 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 oxaflufen-ethyl. Background technique [0002] Ethoxyfenapyr, the chemical name is (R)-2-[4-(6-chloro-2-benzoxazolyloxy)phenoxy]propionic acid ethyl ester, is a new type of phenoxycarboxylic acid. Ring herbicide, with high efficiency, low toxicity, little environmental pollution, etc; Very good control effect. The traditional reaction process for the synthesis of oxaflufen-ethyl is a solid-liquid phase reaction, and the synthesis method has serious deficiencies, 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, the liquid phase reaction is also used to prepare fenoxafen, but there is a large-scale separation of organic solvents or mixed solvents in the production process. SUMMARY...

Claims

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Application Information

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