Preparation method of 3, 5-dimethyl-4-chlorophenol

A technology of dimethylphenol and chlorophenol, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry and other directions, can solve the problems of increasing the difficulty of post-processing, and achieve the improvement of the conversion rate of the substrate, the simple process flow, and the reduction of The effect of pollution

Active Publication Date: 2021-01-22
ZHEJIANG JINKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method avoids the generation of by-product dimers by reducing the conversion rate of MX, it greatly increases the difficulty of post-processing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation method of embodiment 1,3,5-dimethyl-4-chlorophenol

[0031] Add 122g of 3,5-dimethylphenol (1mol) into a 1000ml three-necked flask, then add 366g of glacial acetic acid, start stirring, start to add 141.8g of sulfuryl chloride (1.05mol) dropwise at 25°C, and control the reaction temperature at 30-35°C ℃, drop time 3h; after the drop is completed, the reaction is terminated, the sample is analyzed by GC, and the results are MX: 0.35%, PCMX: 90.5%, OCMX: 7.4%, DCMX: 1.75%.

[0032] The material was distilled under reduced pressure to remove the solvent glacial acetic acid, and then purified by rectification (control the vacuum degree -0.09Mpa, the kettle temperature was 150°C, and the fraction with a top temperature of 130°C was collected), and 138g of white crystal product was obtained. The GC analysis result was, MX: 0.10%, PCMX: 99.6%, OCMX: 0.22%, DCMX: 0.08%. The yield was 88.1% (molar yield based on MX).

Embodiment 2

[0033] The preparation method of embodiment 2,3,5-dimethyl-4-chlorophenol

[0034] Add 122g of 3,5-dimethylphenol (1mol) into a 1000ml three-necked flask, then add 488g of glacial acetic acid, start stirring, start adding 148.5g of sulfuryl chloride (1.1mol) dropwise at 20°C, and control the reaction temperature at 20-25°C , the dropping time was 4h; after the dropping was completed, the reaction was terminated, and the samples were analyzed by GC, and the results were MX: 0.15%, PCMX: 87.5%, OCMX: 8.4%, and DCMX: 3.95%.

[0035] The material was distilled under reduced pressure to remove the solvent glacial acetic acid, and then purified by rectification to obtain 130 g of a white crystal product. The GC analysis results were: MX: 0.07%, PCMX: 99.43%, OCMX: 0.32%, DCMX: 0.18%. The yield was 83.0% (molar yield based on MX).

Embodiment 3

[0036] The preparation method of embodiment 3,3,5-dimethyl-4-chlorophenol

[0037] Add 122g of 3,5-dimethylphenol (1mol) into a 1000ml three-necked flask, then add 366g of formic acid, start stirring, start to drop 145.8g of sulfuryl chloride (1.08mol) at 20°C, control the reaction temperature at 30-40°C, The dropping time was 2 hours; after the dropping was completed, the reaction was terminated, and the samples were analyzed by GC, and the results were MX: 0.45%, PCMX: 85.52%, OCMX: 11.35%, and DCMX: 2.68%.

[0038] The material was purified by rectification after vacuum distillation to remove the solvent formic acid to obtain 128g of white crystal product. GC analysis results were: MX: 0.15%, PCMX: 99.22%, OCMX: 0.39%, DCMX: 0.24%. The yield was 81.7% (molar yield based on MX).

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Abstract

The invention discloses a preparation method of 3, 5-dimethyl-4-chlorophenol, which comprises the following steps: by using 3, 5-dimethylphenol as a raw material, carrying out low-temperature homogeneous chlorination reaction on 3, 5-dimethylphenol and a chlorinating agent in a solvent at 10-70 DEG C for 2-4 hours according to the molar ratio of the chlorinating agent to 3, 5-dimethylphenol of 1.05-1.1: 1, wherein the chlorinating agent is sulfuric chloride; and after the reaction is finished, rectifying the reaction product to obtain the 3, 5-dimethyl-4-chlorophenol. According to the method,the use of a high-toxicity organic solvent is avoided, and the conversion rate of a primary reaction substrate is improved.

Description

technical field [0001] The invention relates to a preparation method of 3,5-dimethyl-4-chlorophenol. Background technique [0002] 3,5-Dimethyl-4-chlorophenol belongs to the class of antiseptics. It has broad-spectrum and high-efficiency killing and inhibiting effects on various bacteria, and is recognized by the US FDA as the preferred bactericidal drug. 3,5-Dimethyl-4-chlorophenol is widely used in personal care products such as hand sanitizers, soaps, anti-dandruff shampoos, and women's lotions because of its low toxicity and low irritation, which can directly contact with the skin. Since the outbreak of the novel coronavirus, which has caused hundreds of thousands of deaths around the world, people have paid more and more attention to personal hygiene, which provides a huge market for the wide application of 3,5-dimethyl-4-chlorophenol. [0003] The prior art discloses multiple technical schemes for synthesizing 3,5-dimethyl-4-chlorophenol, such as: [0004] U.S. Pate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/62C07C37/74C07C39/28
CPCC07C37/62C07C37/74C07C39/28Y02P20/52
Inventor 殷飞刘小棒魏一帆徐聪张纪光
Owner ZHEJIANG JINKE CHEM
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