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Method for synthesizing intermediate of agricultural bactericide fenoxanil

A technology of an agricultural fungicide and a synthetic method, which is applied in the field of intermediates of the agricultural fungicide rice blastamide, can solve the problems of phenol-containing wastewater discharge, unfavorable popularization and application, etc., and achieve the effects of reducing emissions, complete reaction, and reducing production costs

Inactive Publication Date: 2010-01-13
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Report in EP263393 that this intermediate 2-(2,4-dichlorophenoxy group) propionic acid synthetic method adopts water as medium, and its yield only has about 90%, and the reaction time is 15 hours, also causes a large amount of waste water containing phenol emission, which is not conducive to popularization and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In a 1000ml reaction flask equipped with stirring, a thermometer, and a reflux condenser, add 163g (1mol) 2,4-dichlorophenol, 400ml dimethyl sulfoxide, 109g (1mol) 2-chloropropionic acid, 125g (2mol) Potassium hydroxide and 2g of dimethylaminopyridine were heated to 30°C and stirred for 10 hours. After the reaction was completed, at the bottom temperature of 30°C, sulfuric acid was added dropwise for neutralization, filtered, and the solvent was distilled off under reduced pressure.

[0012] Take 254g of solids, add 635g of n-hexane, stir and cool to room temperature, and filter to obtain 227g of product 2-(2,4-dichlorophenoxy)propionic acid with a yield of 93%.

Embodiment 2

[0014] In a 1000ml reaction flask equipped with stirring, a thermometer, and a reflux condenser, add 163g (1mol) 2,4-dichlorophenol, 400ml dimethyl sulfoxide, 109g (1mol) 2-chloropropionic acid, 125g (2mol) Potassium hydroxide and 4 g of dimethylaminopyridine were stirred at 20°C for 10 hours. After the reaction was completed, sulfuric acid was added dropwise for neutralization, filtered, and the solvent was distilled off under reduced pressure.

[0015] Take 260g of solid matter, add 780g of n-hexane, stir and cool to room temperature, and filter to obtain 227g of product 2-(2,4-dichlorophenoxy)propionic acid, with a yield of 93%.

Embodiment 3

[0017] In a 1000ml reaction flask equipped with stirring, a thermometer, and a reflux condenser, add 163g (1mol) 2,4-dichlorophenol, 300ml dimethyl sulfoxide, 109g (1mol) 2-chloropropionic acid, 125g (2mol) Potassium hydroxide and 1.5 g of dimethylaminopyridine were stirred at 80°C for 8 hours. After the reaction was completed, the temperature was maintained at 80°C, neutralized by adding sulfuric acid dropwise, filtered, and the solvent was distilled off under reduced pressure.

[0018] Take 257g of solid matter, add 550g of n-hexane, stir and cool to room temperature, and filter to obtain 225g of product 2-(2,4-dichlorophenoxy)propionic acid, with a yield of 93.2%.

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PUM

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Abstract

The invention discloses a method for synthesizing the intermediate of agricultural bactericide fenoxanil and relates to a process for synthesizing an agricultural intermediate. The method comprises the following steps: putting 2,4-dichlorophenol, 2-chloropropionic acid, potassium hydroxide and surfactant in a dimethyl sulfoxide solvent, keeping a reaction temperature between 20 and 80 DEG C, keeping the temperature after the reaction is finished, neutralizing the reaction solution with sulfuric acid, filtering the neutralized reaction solution and distilling filtrate at a reduced pressure to remove the solvent; and taking a solid substance, adding normal hexane into the solid substance, cooling the mixture to room temperature, and filtering the mixture to obtain 2-(2,4-dichlorophenoxy) propionic acid. Using a solvent in place of water as a medium, the synthesis method of the invention improves condensation yield to 90 percent, reduces the discharge of water containing phenol during reaction and reduces production cost by recycling the solvent.

Description

technical field [0001] The invention relates to a synthesis process of 2-(2,4-dichlorophenoxy)propionic acid, an intermediate of the agricultural fungicide rice blastamide. Background technique [0002] 2-(2,4-dichlorophenoxy)propionic acid is an important intermediate in the synthesis of the agricultural fungicide blastamide. Blasticamide is widely used to control rice blast, sheath blight, and wheat head blight. Report in EP263393 that this intermediate 2-(2,4-dichlorophenoxy group) propionic acid synthetic method adopts water as medium, and its yield only has about 90%, and the reaction time is 15 hours, also causes a large amount of waste water containing phenol Emissions are not conducive to popularization and application. Contents of the invention [0003] The object of the invention is to provide a short reaction time, high yield, and a synthetic method for the intermediate of the agricultural fungicide rice blastamide that reduces the discharge of phenol-containi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/68C07C51/367
Inventor 于国权吕良忠沈迎春
Owner JIANGSU CHANGQING AGROCHEMICAL CO LTD
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