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Production process of difenoconazole

A technology of difenoconazole and production process, applied in the field of production technology of difenoconazole, can solve problems such as difficulty in achieving quality and yield, air pollution, stimuli, etc., and achieve shortened process reaction time, cleanliness Environmentally friendly production, the effect of improving yield

Inactive Publication Date: 2015-07-29
JIANGSU CHANGQING AGROCHEM NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The weak point of above-mentioned patented method is: 1, in the preparation process of starting material 4-(4-chlorophenoxy group)-2-chloroacetophenone, be difficult to reach ideal quality and yield, cause purification and separation difficult, thus greatly affecting the content of crude difenoconazole
At the same time, the compound has a very irritating effect on the eyes and skin, and is relatively harmful to the operator. Advanced protective equipment should be equipped.
2. In the process of salt formation and neutralization reaction, a large amount of organic solvent is needed, which is lost in the process of recycling organic solvent, which is easy to cause air pollution
In addition, during the washing process, a large amount of wastewater is generated, which is difficult to treat and discharge up to the standard

Method used

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  • Production process of difenoconazole
  • Production process of difenoconazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The production technology of difenoconazole comprises the following steps:

[0031] a. Etherification: Put the weighed p-chlorophenol, solid potassium hydroxide and measured m-dichlorobenzene into the etherification reaction kettle, heat up the jacket steam to 100°C, and perform dehydration reaction at normal pressure for 10 hours. After sampling and analysis are qualified , the cooling water drops to room temperature and then filtered, the filter residue containing potassium chloride is sent to solid waste treatment, the filtrate is returned to the reaction kettle and the jacket is heated to 140°C, first at normal pressure and then depressurized to -0.090 MPa to remove excess m-dichloride Benzene is recovered and used mechanically, and the etherified compound obtained is transferred to the next process;

[0032] b. Acylation: At room temperature, add the etherified product obtained in the previous step, a small amount of aluminum trichloride and metered dichloromethane...

Embodiment 2

[0037] The production technology of difenoconazole comprises the following steps:

[0038] a. Etherification: Put the weighed p-chlorophenol, solid potassium hydroxide and measured m-dichlorobenzene into the etherification reaction kettle, heat up the jacketed steam to 102°C, and perform dehydration reaction under normal pressure for 11 hours. After sampling and analysis are qualified , the cooling water drops to room temperature and then filtered, the filter residue containing potassium chloride is sent to solid waste treatment, the filtrate is returned to the reaction kettle and the jacket is heated to 140°C, first at normal pressure and then decompressed to -0.091 MPa to remove excess m-dichloride Benzene is recovered and used mechanically, and the etherified compound obtained is transferred to the next process;

[0039] b. Acylation: At room temperature, add the etherified product obtained in the previous step, a small amount of aluminum trichloride and metered dichloromet...

Embodiment 3

[0044] The production technology of difenoconazole comprises the following steps:

[0045] a. Etherification: Put the weighed p-chlorophenol, solid potassium hydroxide and measured m-dichlorobenzene into the etherification reaction kettle, heat up the jacket steam to 105°C, and perform dehydration reaction under normal pressure for 12 hours. After sampling and analysis are qualified , the cooling water drops to room temperature and then filtered, the filter residue containing potassium chloride is sent to solid waste treatment, the filtrate is returned to the reaction kettle and the jacket is heated to 142°C, first at normal pressure and then depressurized to -0.092MPa to remove excess m-dichloride Benzene is recovered and used mechanically, and the etherified compound obtained is transferred to the next process;

[0046] b. Acylation: At room temperature, add the etherified product obtained in the previous step, a small amount of aluminum trichloride and metered dichlorometha...

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Abstract

The invention discloses a production process of difenoconazole. The production process comprises steps as follows: etherification: parachlorophenol and solid potassium hydroxide which are well weighed and metered m-dichlorobenzene are put into an etherification reaction kettle, and etherate is obtained and transferred to a next procedure; acylation: etherate obtained in the etherification step, a small amount of aluminum trichloride and metered methylene dichloride are added to an acylation kettle to be stirred and mixed at the room temperature, acetyl chloride is dropwise added for a reaction, and acylate is obtained and transferred to a next procedure; cyclization: acylate obtained in the acylation step as well as propylene glycol and cyclohexane which are metered is put into a cyclization kettle at the room temperature, and materials are transferred to a next procedure after the materials are cooled to the room temperature by cooling water; bromination: a cyclization material is introduced into a bromination kettle at the room temperature, is bromized by dropwise adding bromine and is added with water for washing, waste water obtained through washing is sent for waste water treatment, and bromide is obtained and transferred to a next procedure; condensation: the bromide obtained in the bromination step, triazole, caustic soda flakes and dimethyl sulfoxide are put into a condensation reaction kettle. According to the production process of the difenoconazole, the reaction time of the process is shortened, the yield is increased, three wastes are fewer, and clean and environment-friendly production is realized.

Description

technical field [0001] The invention relates to a production process of difenoconazole. Background technique [0002] For the production process route of difenoconazole, the patent application document No. 200410065404.5 discloses a synthetic process route as: 4-(4-chlorophenoxy)-2-chloroacetophenone and 1,2- Propylene glycol cyclization reaction to form a cyclic compound-cis, trans-3-chloro-4-(2,4-dimethyl-1,3-dioxolan-2-yl)phenyl-4-chlorophenyl ether , The reaction is in the presence of catalyst p-toluenesulfonic acid in the solvent, the above cyclic compound reacts with bromine to generate bromide-cis, trans-3-chloro-4-(4-methyl-2-bromomethyl- 1,3-dioxolan-2-yl)phenyl-4-chlorophenyl ether; above-mentioned bromide and 1,2,4-triazole sodium, under the catalysis of potassium iodide, react in polar solvent, its The concentration mass ratio is 15%-50%, and the target compound is prepared. [0003] The weak point of above-mentioned patented method is: 1, in the preparation p...

Claims

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Application Information

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IPC IPC(8): C07D405/06
CPCC07D405/06
Inventor 洪晓冬张振明赵晶刘凯
Owner JIANGSU CHANGQING AGROCHEM NANTONG
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