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4-phenoxybenzoic acid synthesis method

A technology of phenoxybenzoic acid and synthesis method, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of product purity, poor color, high cost of raw materials, and many raw materials. To achieve the effect of simple and easy to obtain starting materials, less waste water and cheap starting materials

Inactive Publication Date: 2019-11-05
CHENGWU CHENHUI ENVIRONMENTAL PROTECTION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the industrialized production of 4-phenoxybenzoic acid, most of the technical routes reported in the literature are to use diphenyl ether as the starting material, and obtain the target product through acetylation, haloform reaction, and acidification; the fundamental way is to use a similar halogen There are many similar reports on the synthesis of substituted benzoic acid by imitation method. The above-mentioned production route uses many raw materials, produces a large amount of waste water, and the cost of raw materials is high. The purity and color of the product are not good.
In the prior art, there is no better process with high yield and suitable for industrialized production to be disclosed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of synthetic new technique of 4-phenoxybenzoic acid, its technological process is as follows:

[0027] Add 94.6g of phenol, 61g of sodium hydroxide, and 60g of water into a 250ml flask, heat to 60°C, react for 2.5 hours, take a sample and test until the phenol is almost completely reacted to sodium phenate, and keep the temperature for later use;

[0028] Add 600g of tetrahydronaphthalene and 158.7g of p-chlorobenzoic acid into a 1000ml four-necked flask, add a reflux water separator, heat the system temperature to about 155°C, slowly add a step of sodium phenoxide solution dropwise, along with the dropping After the process, water will gradually evaporate in the water separator, and the dropwise addition will be completed in about 8 hours. After the dropwise addition, the reaction will be kept for 2 hours, and the sample will be tested after treatment. The reaction end point will be less than 0.5% phenol. After the reaction, cool down to 30°C, filter, add the ob...

Embodiment 2

[0031] A kind of synthetic new technique of 4-phenoxybenzoic acid, its technological process is as follows:

[0032] Add 94.6g of phenol, 78g of sodium hydroxide, and 70g of water into a 250ml flask, heat to 60°C, react for 2 hours, take a sample and test until the phenol is almost completely reacted to sodium phenate, keep the temperature for later use;

[0033] Add 530g tetrahydronaphthalene and 158.7g p-chlorobenzoic acid into a 1000ml four-necked flask, add a reflux water separator, heat the system temperature to about 150°C, slowly add a step of sodium phenoxide solution dropwise, along with the dropping After the process, water will gradually evaporate in the water separator, and the dropwise addition will be completed in about 8 hours. After the dropwise addition, the reaction will be kept for 2 hours, and the sample will be tested after treatment. The reaction end point will be less than 0.5% phenol. After the reaction, cool down to 30°C, filter, add the obtained solid...

Embodiment 3

[0036] A kind of synthetic new technique of 4-phenoxybenzoic acid, its technological process is as follows:

[0037] Add 94.6g of phenol, 50g of sodium hydroxide, and 60g of water into a 250ml flask, heat to 60°C, react for 3 hours, take a sample and test, it is known that phenol is basically completely reacted to sodium phenate, keep the temperature for later use;

[0038] Add 650g of tetrahydronaphthalene and 158.7g of p-chlorobenzoic acid into a 1000ml four-necked flask, add a reflux water separator, heat the system temperature to 160°C, slowly add a step of sodium phenoxide solution dropwise, as the dropwise addition proceeds , water will gradually evaporate out of the water separator, about 8h after the dropwise addition, after the dropwise addition, keep warm for 2h, after sampling and treatment, test, and the reaction end point is less than 0.5% phenol. After the reaction, cool down to 30°C, filter, add the obtained solid to a 1000ml flask, add 500ml of water to stir, b...

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Abstract

The invention relates to the technical field of chemical industry synthesis, and particularly discloses a 4-phenoxybenzoic acid synthesis method, which comprises: carrying out a mixing heating reaction on phenol as a raw material, sodium hydroxide and water to obtain a sodium phenolate solution; slowly adding the sodium phenolate solution into a mixture of tetrahydronaphthalene and p-chlorobenzoicacid in a dropwise manner while heating, and carrying out a thermal insulation reaction; after completing the reaction, cooling the reaction liquid, filtering, washing the obtained solid, filtering,mixing by adding clear water, adjusting the pH value, and filtering to obtain crude and wet 4-phenoxybenzoic acid; and dissolving the crude and wet 4-phenoxybenzoic acid in ethanol, adsorbing with active carbon, filtering, cooling, and filtering to obtain the product. According to the present invention, the process route is simple and easy to operate, the reaction can be completed in one step, thestarting raw material is simple and cheap, and is easy to obtain, the generated waste water is less, and the method is suitable for industrial production, and is a completely-new synthesis route.

Description

[0001] (1) Technical field [0002] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing 4-phenoxybenzoic acid. [0003] (2) Background technology [0004] 4-Phenoxybenzoic acid has a molecular formula of C13H9O3 and a molecular weight of 213.2093. It can not only be used as an intermediate of medicine and pesticide, but also widely used in ester liquid crystals and high temperature resistant materials. Slotta and Scremba synthesized this compound from 4-phenoxybenzaldehyde for the first time through oxidation. Litter et al. used potassium hypochlorite to oxidize 4-phenoxy ketone to synthesize 4-phenoxybenzoic acid (64% yield). [0005] At present, the industrialized production of 4-phenoxybenzoic acid, most of the technical routes reported in the literature are to use diphenyl ether as the starting material, and obtain the target product through acetylation, haloform reaction, and acidification; the fundamental way is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/92
CPCC07C67/31C07C69/92
Inventor 陈宏平崔礼龙李守峰
Owner CHENGWU CHENHUI ENVIRONMENTAL PROTECTION TECH CO LTD
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