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Synthesis and preparation process of 4-phenoxybenzoic acid

A technology of phenoxybenzoic acid and preparation process, which is applied in the directions of oxidative preparation of carboxylic acid, condensation preparation of carbonyl compounds, organic chemistry, etc. The effect of improving the reaction rate and product yield

Inactive Publication Date: 2020-02-18
上海星酶生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] A synthesis and preparation process of 4-phenoxybenzoic acid proposed by the present invention solves the problem that there is no obvious guarantee for the yield and many residues will appear in the production process

Method used

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  • Synthesis and preparation process of 4-phenoxybenzoic acid

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Comparison scheme
Effect test

Embodiment 1

[0022] A kind of synthetic preparation technology of 4-phenoxybenzoic acid, comprises following preparation steps:

[0023] Step 1: Select an appropriate amount of diphenyl ether and dichloromethane into the same reactor, then add anhydrous aluminum trichloride solution to the reactor for stirring, stir for 30 minutes and then add acetic anhydride, heat the reactor and continue stirring , the reactor was continuously heated for 3h, and the stirring rate during the heating process was 25r / min;

[0024] Step 2: Add ice water to the reactor and stir. The ice water and the original solution in the reactor are added in a ratio of 1:3. After stirring, the solution is added to the concentration equipment for concentration treatment. After the treatment is completed, it is passed into the distillation equipment for further processing. Distillation treatment, the distillation temperature is kept at 48 ° C, and the distillation is continued for 35 minutes. The dichloromethane and the or...

Embodiment 2

[0029] A kind of synthetic preparation technology of 4-phenoxybenzoic acid, comprises following preparation steps:

[0030] Step 1: Select an appropriate amount of diphenyl ether and methylene chloride and add them to the same reactor, then add anhydrous aluminum trichloride solution to the reactor for stirring, after stirring for 50 minutes, add acetic anhydride, heat the reactor and continue stirring , the reactor was continuously heated for 5h, and the stirring rate during the heating process was 45r / min;

[0031] Step 2: Add ice water to the reactor and stir. The ice water and the original solution in the reactor are added in a ratio of 1:5. After stirring, the solution is added to the concentration equipment for concentration treatment. After the treatment is completed, it is passed into the distillation equipment for further processing. Distillation treatment, the distillation temperature is kept at 56 ° C, and the distillation is continued for 55 minutes. The dichlorome...

Embodiment 3

[0036] A kind of synthetic preparation technology of 4-phenoxybenzoic acid, comprises following preparation steps:

[0037] Step 1: Select an appropriate amount of diphenyl ether and methylene chloride and add them to the same reactor, then add anhydrous aluminum trichloride solution to the reactor for stirring, stir for 40 minutes and then add acetic anhydride, heat the reactor and continue stirring , the reactor was continuously heated for 4h, and the stirring rate during the heating process was 35r / min;

[0038] Step 2: Add ice water to the reactor and stir. The ice water and the original solution in the reactor are added in a ratio of 1:4. After stirring, the solution is added to the concentration equipment for concentration treatment. After the treatment is completed, it is passed into the distillation equipment for further processing. Distillation treatment, the distillation temperature is kept at 52 ° C, and the distillation is continued for 45 minutes. The dichlorometh...

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Abstract

The invention belongs to the field of compound production, and in particular, relates to a synthesis and preparation process of 4-phenoxybenzoic acid. According to the technical scheme, the preparation method comprises the following preparation steps: step 1, selecting a proper amount of diphenyl ether and dichloromethane, adding diphenyl ether and dichloromethane into a same reactor, then addingan anhydrous aluminum trichloride solution into the reactor, stirring for 30-50 min, then adding acetic anhydride, and heating and continuously stirring in the reactor; and step 2, adding ice water into the reactor and stirring, and adding the solution into concentration equipment after stirring, and carrying out concentration treatment. In the preparation process, hydrochloric acid is used for monitoring and adjusting the pH value of the solution, the pH value is maintained at about 7, and stirring and processing are performed, so that the whole reaction rate can be accelerated, the reactioncan be completely performed, the residue is less, the product yield is significantly improved, the dichloromethane with high purity can be extracted through the distillation processing so as to be reused in the subsequent steps, and the energy saving and the environmental protection are achieved.

Description

technical field [0001] The invention relates to the technical field of compound production, in particular to a synthesis and preparation process of 4-phenoxybenzoic acid. Background technique [0002] 4-Benzyloxybenzoic acid is a chemical substance with the molecular formula C 14 h 11 o 3 , 4-phenoxybenzoic acid can not only be used as an intermediate of pharmaceuticals and pesticides, but also widely used in ester liquid crystals and high temperature resistant materials. Slotta and Soremball were first prepared by oxidation of 4-phenoxybenzaldehyde This compound, the way that is often used at present is to use potassium hypochlorite to oxidize 4-phenoxyacetophenone to synthesize 4-phenoxybenzoic acid (yield rate is 64%), or adopt the method for synthesizing substituted benzoic acid similar to the haloform method More, but this kind of method does not have obvious guarantee to the productive rate of 4-phenoxybenzoic acid, and there will be more residue in the production p...

Claims

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Application Information

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IPC IPC(8): C07C51/16C07C65/24
CPCC07C45/46C07C51/16C07C49/84C07C65/24
Inventor 陈艳辉
Owner 上海星酶生物科技有限公司
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