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Preparation method of 4-chloro-4'-hydroxybenzophenone

A technology for hydroxybenzophenone and p-chlorobenzonitrile, which is applied in the field of compound preparation, can solve the problems of high industrialization cost, difficult source of raw materials, complicated routes, etc., and achieves the effects of low cost, simple reaction and easy recovery.

Inactive Publication Date: 2018-03-09
江苏万隆科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are multiple preparation methods for 4-chloro-4'-hydroxybenzophenone, but there are difficulties in the source of raw materials, complex routes, low yield, and high industrialization costs.

Method used

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  • Preparation method of 4-chloro-4'-hydroxybenzophenone

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Experimental program
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Effect test

Embodiment 1

[0015] The specific steps of the preparation method of 4-chloro-4'-hydroxybenzophenone in this embodiment include: adding 500 ml of dichloroethane, 100 g of phenol, 146 g of p-chlorobenzonitrile, and 20 g of anhydrous zinc chloride into the reaction kettle Stir with 5g of Dowex 50W resin produced by Dow Chemical, and control the temperature at 95°C to continuously feed dry hydrogen chloride gas. During the ventilation process, the reaction of the material is detected intermittently until the p-chlorobenzonitrile is completely reacted. Cool to room temperature and add concentration. It is 400ml of 30% hydrochloric acid aqueous solution, heated to reflux, reacted for 6h, until the hydrolysis of the intermediate is completed, then cooled to room temperature, layered, washed with water, dichloroethane is recovered from the organic layer, and the residue is added with 15% sodium hydroxide Dissolve 200ml of the aqueous solution, decolorize with 8g of activated carbon, acidify, filter...

Embodiment 2

[0019] The specific steps of the preparation method of 4-chloro-4'-hydroxybenzophenone in this embodiment include: adding 600 ml of dichloroethane, 120 g of phenol, 146 g of p-chlorobenzonitrile, and 25 g of anhydrous zinc chloride into the reaction kettle Stir with 8g of Dowex 50W resin produced by Dow Chemical, and control the temperature at 90°C to continuously feed dry hydrogen chloride gas. During the ventilation process, check the reaction of the material until the p-chlorobenzonitrile is completely reacted. Cool to room temperature and add concentration. It is 500ml of 30% hydrochloric acid aqueous solution, heated to reflux, reacted for 5h, until the hydrolysis of the intermediate is completed, then cooled to room temperature, layered, washed with water, dichloroethane is recovered from the organic layer, and the residue is added with 15% sodium hydroxide 250ml of the aqueous solution was dissolved, decolorized with 8g of activated carbon, acid-precipitated, suction fil...

Embodiment 3

[0021] The specific steps of the preparation method of 4-chloro-4'-hydroxybenzophenone in this embodiment include: adding 550 ml of dichloroethane, 120 g of phenol, 146 g of p-chlorobenzonitrile, and 22 g of anhydrous zinc chloride into the reaction kettle Stir with 7g of Dowex 50W resin produced by Dow Chemical, and control the temperature at 90°C to continuously feed dry hydrogen chloride gas. During the ventilation process, check the reaction of the material until the p-chlorobenzonitrile is completely reacted. Cool to room temperature and add concentration. It is 450ml of 30% hydrochloric acid aqueous solution, heated to reflux, reacted for 7h, until the hydrolysis of the intermediate is completed, then cooled to room temperature, layered, washed with water, dichloroethane is recovered from the organic layer, and the residue is added with 15% sodium hydroxide Dissolve 200 ml of the aqueous solution, decolorize with 8 g of activated carbon, acidify, filter with suction, and ...

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Abstract

The invention relates to a preparation method of 4-chloro-4'-hydroxybenzophenone. The preparation method comprises the following steps: adding a proper amount of dichloroethane, phenol, 4-chlorobenzonitrile, anhydrous zinc chloride and gel type strong-acid ion exchange resin into a reaction kettle and stirring; controlling temperature to 50 DEG C to 120 DEG C and continuously introducing dry hydrogen chloride gas until the 4-chlorobenzonitrile reacts completely; cooling to room temperature and adding a proper amount of a hydrochloric acid solution; raising the temperature, reflowing and reacting for 5h to 7h; then cooling to room temperature and layering; recycling the dichloroethane into an organic layer and adding alkali into residues and dissolving; de-coloring by utilizing active carbon, carrying out acid precipitation, extracting and filtering and drying to obtain the 4-chloro-4'-hydroxybenzophenone. The preparation method of the 4-chloro-4'-hydroxybenzophenone, provided by the invention, is simple in route and high in yield.

Description

technical field [0001] The present invention relates to a kind of preparation method of compound, especially a kind of preparation method of 4-chloro-4'-hydroxybenzophenone. Background technique [0002] 4-Chloro-4'-hydroxybenzophenone is an important pharmaceutical intermediate. There are various preparation methods of 4-chloro-4'-hydroxybenzophenone, but all have the disadvantages of difficult source of raw materials, complicated route, low yield, and high industrialization cost. . [0003] How to provide a preparation method of 4-chloro-4'-hydroxybenzophenone with a simple route and high yield is a technical problem to be solved by those skilled in the art. SUMMARY OF THE INVENTION [0004] The technical problem to be solved by the present invention is to provide a preparation method of 4-chloro-4'-hydroxybenzophenone with a simple route and high yield. [0005] A technical scheme proposed by the present invention to solve the above-mentioned technical problems is: a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/44C07C49/83
CPCC07C45/44C07C49/83
Inventor 吴勇才
Owner 江苏万隆科技有限公司
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