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Preparation method of dichlorodiphenylene ether ketone

A technology of dichlorodiphenyl ether ketone and dichlorodiphenyl ether, which is applied in the field of preparation of dichlorodiphenyl ether ketone, can solve the problems of low recycling rate of waste liquid, harsh reaction conditions, large discharge of three wastes, etc. The effect of high liquid recycling rate, short synthesis route and less discharge of three wastes

Inactive Publication Date: 2013-05-01
扬州市天平化工厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the dichlorodiphenyl ether ketone synthesized by the prior art mainly has the following disadvantages: the synthesis route is long and complicated, the reaction conditions are harsh, the conversion rate is low, the production cost is high, the discharge of three wastes is large, and the recycling rate of waste liquid is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A preparation method of dichlorodiphenyl ether ketone, comprising the following steps:

[0016] (1) Condensation reaction: Add 225 kg of p-chlorophenol and 300 kg of 50% sodium hydroxide solution to make phenoxide into a 3000 L reaction pot, then add 720 kg of toluene to reflux to remove water, and control the reflux temperature to 107°C. At the end of water removal, distill toluene, and steam to an internal temperature of 115°C, then cool down to room temperature, add 50 kg of copper acetate catalyst, 100 kg of diethylacetamide, and 800 kg of m-dichlorobenzene, raise the temperature to 148°C, keep it for 48 hours, and measure The conversion rate is 96% qualified, cooled to room temperature and filtered to remove the copper acetate catalyst, the filter cake was washed with water, the waste water layer was discarded, the oil layer was distilled under reduced pressure, m-dichlorobenzene was recovered and recycled, steamed to an internal temperature of 180°C, and cooled to ...

Embodiment 2

[0020] A preparation method of dichlorodiphenyl ether ketone, comprising the following steps:

[0021] (1) Condensation reaction: Add 225 kg of p-chlorophenol and 225 kg of 50% sodium hydroxide solution to make phenoxide into a 3000 L reaction pot, then add 700 kg of toluene to reflux to remove water, and control the reflux temperature to 105°C. At the end of water removal, distill off toluene, steam to an internal temperature of 115°C, cool down to room temperature, add 22.5 kg of copper acetate catalyst, 45 kg of diethylacetamide and 675 kg of m-dichlorobenzene, raise the temperature to 150°C, keep it for 45 hours, and measure The conversion rate is 96% qualified, cooled to room temperature and filtered to remove the copper acetate catalyst, the filter cake was washed with water, the waste water layer was discarded, the oil layer was distilled under reduced pressure, m-dichlorobenzene was recovered and recycled, steamed to an internal temperature of 180°C, and cooled to Tran...

Embodiment 3

[0025] A preparation method of dichlorodiphenyl ether ketone, comprising the following steps:

[0026] (1) Condensation reaction: add 225 kg of p-chlorophenol and 337.5 kg of 50% sodium hydroxide solution into a 3000 L reaction pot to make phenoxide, then add 750 kg of toluene to reflux to remove water, and control the reflux temperature to 110°C. At the end of water removal, distill off toluene, and steam to an internal temperature of 115°C. After cooling down to room temperature, add 90 kg of copper acetate catalyst, 135 kg of diethylacetamide and 900 kg of m-dichlorobenzene, raise the temperature to 152°C, and keep it for 50 h. The conversion rate is 96% qualified, cooled to room temperature and filtered to remove the copper acetate catalyst, the filter cake was washed with water, the waste water layer was discarded, the oil layer was distilled under reduced pressure, m-dichlorobenzene was recovered and recycled, steamed to an internal temperature of 180°C, and cooled to Tr...

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Abstract

The invention discloses a preparation method of dichlorodiphenylene ether ketone. The method includes the steps as follows: (1) condensation reaction: adding p-chlorophenol and a sodium hydroxide solution into a reactor to prepare phenoxide; dehydrating and adding a copper acetate catalyst, assistants and m-dichlorobenzene; and subjecting phenoxide to a condensation reaction with m-dichlorobenzene under the effects of the copper acetate catalyst and the assistants to prepare dichlordiphenyl ether; (2) acylation reaction: dissolving the prepared dichlordiphenyl ether in a solvent, and then subjecting dichlordiphenyl ether to an acylation reaction under the catalysis of an anhydrous aluminum trichloride catalyst to generate dichlorodiphenylene ether ketone. The preparation method has the advantages of short and simple synthetic route, mild reaction conditions, high conversion rate, low production cost, little discharge of three wastes, and high waste liquor recycling rate.

Description

technical field [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to a preparation method of dichlorodiphenyl ether ketone. Background technique [0002] Dichlorodiphenyl ether ketone is an important intermediate of pesticide fungicides, imidazoles, tricyclazoles, etc. However, the dichlorodiphenyl ether ketone synthesized by the prior art mainly has the following disadvantages: the synthesis route is long and complicated, the reaction conditions are harsh, the conversion rate is low, the production cost is high, the discharge of three wastes is large, and the recycling rate of waste liquid is low. Contents of the invention [0003] The technical problem mainly solved by the present invention is to provide a preparation method of dichlorodiphenyl ether ketone with short and simple synthesis route, mild reaction conditions, high conversion rate, low production cost, less discharge of three wastes, and high waste liquid r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/46
Inventor 吕欢欢马文元张兴华
Owner 扬州市天平化工厂有限公司
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