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Catalytic synthesis method of difenoconazole intermediate phenyl ether ketone

A technology for difenoconazole and diphenoxide, which is applied in the field of organic synthesis and can solve the problems of unfavorable industrial production, low product yield and high impurity content

Pending Publication Date: 2021-12-31
山东潍坊双星农药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above defects, the purpose of the present invention is to provide a catalytic synthesis method of difenoconazole intermediate phenylether ketone, which aims to solve the problem of high impurity content, low product yield and pollution in the synthesis process of phenylether ketone in the prior art. Environmental, high cost and technical issues that are not conducive to industrial production

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  • Catalytic synthesis method of difenoconazole intermediate phenyl ether ketone
  • Catalytic synthesis method of difenoconazole intermediate phenyl ether ketone

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preparation example Construction

[0024] The invention provides a catalytic synthesis method of difenoconazole intermediate difenoconazole, comprising the following steps:

[0025] Step 1. Mix 3,4'-dichlorodiphenyl ether and acetyl chloride in a molar ratio of 1:1.05~1.1, and dichloroethane and diphenyl ether in a weight ratio of 3:1, then put them into the configuration kettle, stir and heat up , the material is transferred to the holding kettle for standby;

[0026] Step 2. Control and keep the temperature of the kettle stable. The material is pumped to the top of the reaction tower to distribute evenly through the circulating pump, and then undergoes a Friedel-Crafts reaction with the catalyst on the tray, and then enters the holding kettle through the bottom of the reaction tower, and circulates for 5-6 hours to detect diphenyl ether. When the content is ≤0.5%, the reaction is complete;

[0027] Step 3. Precipitating the reacted material under normal pressure and reduced pressure, adding a refined solvent...

Embodiment 1

[0033] According to the ratio of 3,4'-dichlorodiphenyl ether (referred to as diphenyl ether) and acetyl chloride in a molar ratio of 1:1.05, the ratio of dichloroethane to diphenyl ether in a weight ratio of 3:1 is used for feeding. In the configuration kettle, stir and heat up to 40°C; through the feeding pump, beat the material in the configuration kettle into the holding kettle; pass steam into the holding kettle to control the temperature at 40°C, turn on the circulation pump, and transfer the material from the holding kettle The bottom is blown to the top of the reaction tower, evenly distributed through the top distributor, and passed down through the crystal-like AlCl 3 foam SiC trays, with AlCl 3 Full contact occurs Friedel-Crafts reaction, and then enters the holding tank from the bottom of the reaction tower. Circulate in this way for 4 hours, and take a sample through the detection port for detection. When the content of diphenyl ether is ≤0.5%, the reaction is com...

Embodiment 2

[0036] According to the ratio of 3,4'-dichlorodiphenyl ether (referred to as diphenyl ether) and acetyl chloride molar ratio of 1:1, the ratio of dichloroethane to diphenyl ether is 2:1. In the configuration kettle, stir and heat up to 50°C; through the feeding pump, beat the material in the configuration kettle into the holding kettle; pass steam into the holding kettle to control the temperature at 50°C, turn on the circulation pump, and transfer the material from the holding kettle The bottom is blown to the top of the reaction tower, evenly distributed through the top distributor, and passed down through the crystal-like AlCl 3 foam SiC trays, with AlCl 3 Full contact occurs Friedel-Crafts reaction, and then enters the holding tank from the bottom of the reaction tower. Circulate like this for 6 hours, and take a sample through the detection port for detection. When the content of diphenyl ether is ≤0.5%, the reaction is complete.

[0037] Pump the reacted material into ...

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Abstract

The invention discloses a catalytic synthesis method of difenoconazole intermediate phenyl ether ketone, and relates to the technical field of organic synthesis, wherein the catalytic synthesis method comprises the following steps: step 1, mixing 3,4'-dichlorodiphenyl ether and acetyl chloride according to a molar ratio of 1:(1.05-1), mixing dichloroethane and diphenyl ether according to a weight ratio of 3:1, putting the mixture into a preparation kettle, stirring and heating, and transferring the material into a holding kettle for later use; step 2, controlling the temperature in the kettle to be stable, pumping the material to the top of the reaction tower through a circulating pump, uniformly distributing the material, carrying out Friedel-Crafts reaction on the material and a catalyst on a tower plate, enabling the product to enter a maintaining kettle through the bottom of the reaction tower, circulating for 5-6 hours, and finishing the reaction when the content of diphenyl ether is detected to be less than or equal to 0.5%; and step 3, performing normal-pressure and reduced-pressure desolvation on the reacted material, adding a refining solvent, heating, after the material is completely dissolved, cooling and crystallizing, keeping for 1-2 hours, and centrifuging and drying the material to obtain the phenyl ether ketone. According to the method, salt-containing waste acid is not generated in the synthesis process, impurities are few, the product content is high, the yield is high, and the method is economical, environmentally friendly and suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a catalytic synthesis method of difenoconazole intermediate difenoconazole. Background technique [0002] Difenoconazole (2-chloro-4-(4-chlorophenoxy)acetophenone) is an important pharmaceutical intermediate and the key to the success of the synthetic agricultural fungicide difenoconazole (difenoconazole) where. Difenoconazole is a triazole fungicide widely used and respected in the world. It can strongly inhibit the formation of spores of plant pathogenic bacteria. It has three functions of prevention, treatment and eradication in the process of disease prevention and control. It ranks first among the triazole fungicides and has a great application prospect. [0003] In the research on the synthesis of phenylether ketone, the usual reaction process is to dissolve dichlorodiphenyl ether in a solvent, and under the catalysis of anhydrous aluminum trichloride, undergo a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C49/84
CPCC07C45/46C07C49/84
Inventor 王振江王锡峰公艳茹李大召张孝鹏
Owner 山东潍坊双星农药有限公司