Preparation method for 4, 4-DCDPE (dicarboxydiphenyl ether)

A technology for dicarboxydiphenyl ether and diphenyl ether, which is applied in the field of preparation of 4,4-dicarboxydiphenyl ether, can solve the problems of inapplicable medical intermediates, dark appearance of finished products, complicated synthesis routes, etc., and achieves a simple route. Feasible, white appearance, high purity effect

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

[0002] 4. 4-Dicarboxydiphenyl ether is a class of intermediates that promote metabolism and soften blood vessels. There are few domestic reports, and the synthesis route is complicated, the conditions are harsh, the preparation is difficult, the discharge of three wastes is large, and the finished product has a dark color. , low purity, not suitable for medical intermediates

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of 4,4-dicarboxy diphenyl ether preparation method, comprises the following steps:

[0020] (1) Acylation reaction: Add 480 kg of dichloroethane organic solvent into a 1000 L reaction pot, add 240 kg of anhydrous aluminum trichloride catalyst under stirring, control the temperature below -5°C, and add ethyl alcohol dropwise at the same time Acyl chloride 150 kg, after the dropwise addition, add 100 kg of diphenyl ether dropwise after stirring for 0.5 h, control the temperature in the reaction pot to be less than or equal to 0°C, after the dropwise addition, keep warm for 8 h, measure the conversion rate, the conversion rate is greater than 99% and there is no single When ketone is used, the reaction solution is pumped into 1000 kg of ice water containing hydrochloric acid with a concentration of 10% hydrochloric acid by weight, the temperature is controlled to be less than or equal to 40°C, and the stirring is completed. Wash with water until neutral, remove the ...

Embodiment 2

[0024] A kind of 4,4-dicarboxy diphenyl ether preparation method, comprises the following steps:

[0025] (1) Acylation reaction: Add 450 kg of dichloroethane organic solvent into a 1000 L reaction pot, add 200 kg of anhydrous aluminum trichloride catalyst under stirring, control the temperature below -5°C, and add ethyl alcohol dropwise at the same time Acyl chloride 100 kg, after the dropwise addition, add 100 kg of diphenyl ether dropwise after stirring for 0.3 h, control the temperature in the reaction pot to be less than or equal to 0°C, after the dropwise addition, keep warm for 6 h, measure the conversion rate, the conversion rate is greater than 99% and there is no single When ketone is used, pump the reaction liquid into 800 kg of ice water containing 10% hydrochloric acid by weight, control the temperature to be less than or equal to 40°C and stop stirring, leave to separate after 1.0 h, remove the water layer and the oil layer Wash with water until neutral, remove t...

Embodiment 3

[0029] A kind of 4,4-dicarboxy diphenyl ether preparation method, comprises the following steps:

[0030] (1) Acylation reaction: Add 550 kg of dichloroethane organic solvent into a 1000 L reaction pot, add 300 kg of anhydrous aluminum trichloride catalyst under stirring, control the temperature below -5°C, and add ethyl alcohol dropwise at the same time Acyl chloride 200 kg, after the dropwise addition, after stirring for 1.0 h, add 100 kg of diphenyl ether dropwise, control the temperature in the reaction pot to be less than or equal to 0°C, after the dropwise addition, keep warm for 10 h, measure the conversion rate, the conversion rate is greater than 99% and there is no single When ketone is used, the reaction solution is pumped into 1200 kg of ice water containing hydrochloric acid with a concentration of 10% hydrochloric acid by weight, the temperature is controlled to be less than or equal to 40°C and the stirring is stopped. After 1.5 h, the mixture is allowed to stand...

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Abstract

The invention discloses a preparation method for 4, 4-DCDPE. The method includes the following steps: (1) acylation reaction: adding an organic solvent into a reactor, adding a catalyst with stirring, controlling the temperature to be lower than subzero 5 DEG C, adding acetyl chloride dropwise simultaneously, then adding diphenyl ether dropwise after finishing the previous addition, controlling the temperature in the reactor, finishing adding dropwise, preserving heat for 6-10h, then pumping a reaction liquid into ice water, stirring, standing and layering, removing the water layer, and removing the organic solvent after washing the oil layer to prepare diketone; and (2) oxidation reaction: mixing the prepared diketone and 1,4-dioxane, then adding a sodium hypochlorite solution, controlling the temperature, stirring at the room temperature for 6-10h after finishing the dropwise sodium hypochlorite solution adding, completing the reaction, performing refrigerated centrifugation, and drying to obtain a finished product. The preparation method is simple and practical in route, mild in condition, practical in production, low in production cost and few in discharge of three wastes; and the prepared finished product is white in color of appearance and high in purity, and can be applied to medical intermediates.

Description

technical field [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to a method for preparing 4,4-dicarboxydiphenyl ether. Background technique [0002] 4. 4-Dicarboxydiphenyl ether is a class of intermediates that promote metabolism and soften blood vessels. There are few domestic reports, and the synthesis route is complicated, the conditions are harsh, the preparation is difficult, the discharge of three wastes is large, and the finished product has a dark color. , low purity, not suitable for medical intermediates. Contents of the invention [0003] The technical problem mainly solved by the present invention is to provide a simple and feasible route, mild conditions, feasible production, low production cost, less discharge of three wastes, and the finished product has white appearance and high purity, and can be used for 4, 4- The preparation method of dicarboxy diphenyl ether. [0004] In order to solve the above-...

Claims

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Application Information

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IPC IPC(8): C07C65/24C07C51/16
Inventor吕欢欢马文元张兴华
Owner扬州市天平化工厂有限公司