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Green industrialized preparation method for 1-hydroxy-3,5-dimethyl-chlorobenzene

A technology of dimethylbenzene and dimethyl, which is applied in the field of 1-hydroxyl-3, can solve the problems of high cost and environmental pollution, and can not solve the problems of catalyst recovery and application, so as to avoid the use and production of organic solvents and catalysts. Low cost and the effect of reducing the discharge of three wastes

Active Publication Date: 2010-09-08
湖南瑞冠生物化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still does not solve the recovery and application of catalysts and the use of organic solvents.
[0007] Therefore, when the prior art personnel improve this reaction, they all focus on how to select the catalyst and select the organic solvent, and the resulting cost and environmental pollution remain high.

Method used

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  • Green industrialized preparation method for 1-hydroxy-3,5-dimethyl-chlorobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]Add 122g of 3,5-dimethylphenol (1.0mol) into a 500ml three-necked flask, then add 366g of tap water, start stirring, and keep warm at 15-25°C. Slowly add 108g of sulfuryl chloride (0.8mol) dropwise at this temperature for 4 hours; after the dropwise addition, raise the temperature to 85°C and add 27g of sulfuryl chloride (0.2mol) dropwise after the reactants are melted. After the reaction, the lower organic phase was removed and analyzed by GC. The results were MX: 0.45%; PCMX 84.57%; OCMX (ortho-chlorinated product): 11.56%; DCMX (di-chlorinated product): 3.42%. After the reaction material was suction-filtered and dried, 125 g of a white crystalline product was obtained. The GC analysis results were: MX: 0.25%; PCMX: 99.00%; OCMX: 0.25%; DCMX: 0.50%. The yield was 79.9% (molar yield based on MX).

Embodiment 2

[0035] Add 122g of 3,5-dimethylphenol (1.0mol) into a 500ml three-necked flask, then add 366g of tap water, start stirring, and keep warm at 25-35°C. Slowly add 81g of sulfuryl chloride (0.6mol) dropwise at this temperature, and the dropping time is 4 hours; mol); after the dropwise addition, the temperature was raised to 85°C and then cooled to 25°C, and then 13.5g of sulfuryl (0.1mol) was added dropwise at 25-35°C. After the reaction, the lower organic phase was removed and analyzed by GC. The results were MX: 0.25%; PCMX 89.68%; OCMX (ortho-chlorinated product): 8.19%; DCMX (di-chlorinated product): 1.88%. After the reaction material was filtered and dried by suction, 135 g of a white crystalline product was obtained. The GC analysis results were: MX: 0.2%; PCMX: 99.23%; OCMX: 0.15%; DCMX: 0.42%. The yield was 86.3% (molar yield based on MX).

Embodiment 3

[0037] The experimental process is the same as in Example 1, except that the dripping of sulfuryl chloride is changed into chlorine gas, and after the reaction is finished, the sample analysis is as follows: MX: 0.46%; PCMX: 86.48%; OCMX: 10.65%; DCMX: 2.41%. After the reaction material was suction-filtered and dried, 130 g of a white crystalline product was obtained. The GC analysis results were: MX: 0.25%; PCMX: 99.07%; OCMX: 0.2%; DCMX: 0.48%. The yield was 83% (molar yield based on MX).

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Abstract

The invention discloses a green industrialized preparation method for 1-hydroxy-3,5-dimethyl-chlorobenzene. Water is used as a solvent; sulfuryl chloride or chlorine is used as a chlorinating agent; and a substrate 1-hydroxy-3,5-dimethyl benzene is subjected to chlorination reaction in a mode of multi-stage temperature control. By using the method, a catalyst with high cost and difficult reclamation can be saved, and the use of an organic solvent can be avoided, so that the discharge of waste gas (volatilization of the organic solvent) and waste substance (the catalyst) can be remarkably reduced during production and the industrialized production of the product is more environmentally-friendly and greener).

Description

technical field [0001] The invention relates to a green industrial preparation method of 1-hydroxyl-3,5-dimethyl-4-chlorobenzene. Background technique [0002] 1-Hydroxy-3,5-dimethyl-4-chlorobenzene (also known as: 4-chloro-3,5-dimethylphenol, CAS number: 88-04-0, English abbreviation: PCMX) is a An important microbicide, as an antibacterial agent, antifungal agent, and disinfectant, it is widely used in industry and cosmetics. It has excellent inhibitory effects on bacteria, molds, and most fungi. In recent years, with the raging of epidemic diseases, people's health awareness has become stronger and stronger. As a traditional low-toxicity disinfectant, 1-hydroxy-3,5-dimethyl-4-chlorobenzene will also have more Great development potential, its structural formula is as follows: [0003] [0004] 1-Hydroxy-3,5-dimethyl-4-chlorobenzene is prepared by electrophilic substitution reaction of sulfuryl chloride and 1-hydroxy-3,5-dimethylbenzene. In 1866, since Dubois reacted ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/28C07C37/62
Inventor 吴飞彭斌胡汉忠
Owner 湖南瑞冠生物化工科技有限公司
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