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Synthesis method of 2-chloro-4-(4-chlorophenoxy)-acetophenone

A technology of chlorophenoxy and synthetic method, which is applied in the field of synthesis of 2-chloro-4-acetophenone, can solve the problems of complex operation, low recovery rate of solvent, low recovery rate of diphenyl ether ketone, etc., and achieve product The effect of high yield, simplified production process, and easy industrial implementation

Pending Publication Date: 2021-12-21
NINGXIA RUITAI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process mainly adopts the method of first hydrolyzing and post-processing the solvent to produce diphenyl ether ketone, the solvent recovery rate is low, and the operation is complicated
Methanol is used as the recrystallization solvent in the recrystallization process. Because methanol still has a certain solubility to diphenyl ether ketone at low temperature, the recovery rate of diphenyl ether ketone is low.

Method used

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  • Synthesis method of 2-chloro-4-(4-chlorophenoxy)-acetophenone
  • Synthesis method of 2-chloro-4-(4-chlorophenoxy)-acetophenone
  • Synthesis method of 2-chloro-4-(4-chlorophenoxy)-acetophenone

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0026] (1) Put 75.0 g of diphenyl ether (98.5%) into a 1000 ml four-necked flask, add 90.2 g of solvent dichloroethane, 49.2 g of catalyst aluminum trichloride, and cool down to 5°C. Prepare a uniform solution of 30.0g acetyl chloride and 90.0g dichloroethane, inject it into the reaction system with a metering pump, control the reaction dripping time for 2 hours, and the holding time for 4 hours. After the heat preservation is completed, a small amount of the reaction solution is hydrolyzed to obtain an oil layer, and the normalized gas spectrum detection shows that the content of diphenyl ether is 0.005%, and the content of diphenyl ether ketone is 95.2%. The synthesis device was changed to a distillation device, and 171.3 g of dichloroethane (95% fraction) was removed under negative pressure conditions, and the residue in the still was 132.7 g of black solid particles.

[0027] (2) Prepare a 1000mL four-neck flask, add 380g of deionized water, 20g of reagent hydrochloric aci...

experiment example 2

[0032] (1) Put 75.0 g (0.3 mol) of diphenyl ether (98.5%) into a 1000 ml four-neck flask, add 132 g (0.9 mol) of o-dichlorobenzene as a solvent, and 49.2 g of aluminum trichloride as a catalyst, and cool down to 5°C. Prepare 30.0g of acetyl chloride and 143g of o-dichlorobenzene to form a uniform solution, use a metering pump to inject into the reaction system, control the reaction dripping time for 2 hours, and the holding time for 4 hours. After the heat preservation is completed, a small amount of the reaction solution is hydrolyzed to obtain an oil layer, and the normalized gas spectrum detection shows that the content of diphenyl ether is 0.003%, and the content of diphenyl ether ketone is 95.9%. The synthesis device was changed to a distillation device, and 264g of o-dichlorobenzene (96% fraction) was removed under negative pressure, and the residue in the still was 136.3g of black solid particles.

[0033] (2) Add 380g of deionized water and 20g of reagent hydrochloric ...

experiment example 3

[0038] (1) Put 75.0 g (0.3 mol) of diphenyl ether (98.5%) into a 1000 ml four-neck flask, add 83.2 g (0.90 mol) of solvent toluene, and 89.9 g of catalyst tin chloride, and cool down to 5°C. Prepare 30.0g acetyl chloride and 82.7g toluene into a homogeneous solution, use a metering pump to inject into the reaction system, control the reaction dripping time for 2 hours, and the holding time for 4 hours. After the heat preservation is completed, a small amount of the reaction solution is hydrolyzed to obtain an oil layer, and the normalized gas spectrum detection shows that the content of diphenyl ether is 0.008%, and the content of diphenyl ether ketone is 94.9%. The synthesis device was changed to a distillation device, and 157.6 g of toluene (95% cut) was removed under negative pressure conditions, and the residue in the still was 174.3 g of black solid particles.

[0039] (2) Add 380g of deionized water and 20g of reagent hydrochloric acid into a 1000mL four-neck flask, cool...

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Abstract

The invention discloses a synthesis method of 2-chloro-4-(4-chlorophenoxy)-acetophenone, which comprises the following steps: (1) adding diphenyl ether, Lewis acid and an acetyl chloride solution into a solvent to generate a diphenyl ether ketone synthesis solution; (2) heating the diphenyl ether ketone synthetic liquid to remove a solvent, separating out a solid, reusing the removed solvent in the step (1), adding deionized water into the generated solid, hydrolyzing, and layering to obtain an oil layer and a water layer; (3) washing the oil layer in the step (2) with deionized water once, combining the water after washing with water and the water layer after hydrolysis in the step (2), putting into a kettle, evaporating the oil layer after extraction at the temperature of 50-100 DEG C to recover the solvent, combining the kettle residue obtained after evaporation with the oil layer after washing in the step (3), recrystallizing, and carrying out suction filtration to obtain high-quality diphenyl ether. The production process is simplified, the product yield is high, the raw material consumption is low, and industrial implementation is easy.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a synthesis method of 2-chloro-4-(4-chlorophenoxy)-acetophenone. Background technique [0002] 2-Chloro-4-(4-chlorophenoxy)-acetophenone (hereinafter referred to as "diphenyl ether ketone") is an intermediate for the synthesis of agricultural difenoconazole. Difenoconazole is an ultra-efficient, spectral, and systemic triazole fungicide, which has a strong inhibitory effect on the spore formation of plant pathogenic bacteria, and in the process of preventing and controlling diseases, it shows the three functions of prevention, treatment, and eradication. Great effect. Therefore, its application technology has become the research focus of pesticide companies, and the potential application market is very broad. At present, the use of triazole fungicides in my country is increasing year by year, so stepping up the research and development of its intermediate diphenyl ether ketone and making i...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C45/46C07C45/78C07C45/80C07C45/81C07C49/84
CPCC07C45/455C07C45/46C07C45/78C07C45/80C07C45/81C07C49/84
Inventor 刘勇林洋石苏洋廖强龚正福雍晨阳马荣慧韩小文
Owner NINGXIA RUITAI TECH
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