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1-hydroxyl-3,5-dimethyl-4-chlorobenzene preparation method

A technology of dimethylbenzene and dimethyl, applied in the field of 1-hydroxy-3, can solve the problems of low conversion rate, low para-selectivity, environmental pollution, etc., achieve high conversion rate, reduce environmental pollution, select good sex effect

Active Publication Date: 2012-06-27
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

[0009] In order to overcome the shortcomings of existing production methods such as serious environmental pollution, low para-selectivity, and low conversion rate, the invention provides a method for preparing 1-hydroxy-3,5-dimethyl-4-chlorobenzene, The method is:

Method used

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  • 1-hydroxyl-3,5-dimethyl-4-chlorobenzene preparation method

Examples

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Embodiment 1

[0026] In the 500ml three-necked reaction flask, add 122g (1.0mol) 1-hydroxyl-3,5-dimethylbenzene, 122g acetic acid, 51.2g (0.3) copper chloride dihydrate, 122g tetrachloroethylene, and 102g concentrated hydrochloric acid respectively in the 500ml three-necked reaction flask; Install the condenser, magnetic stirrer, thermometer, and oxygen tube. The reactant was heated to 80°C, and oxygen gas was passed in at a constant speed while stirring. The reaction temperature is controlled between 80-90° C., and the reaction pressure is normal pressure. After the reaction, the lower layer material was separated, and the content was detected by GC. The results are shown in Table 1.

Embodiment 2

[0028]The upper layer water sample in Example 1 was concentrated by atmospheric distillation, and about 100 g of water (containing about 10% acetic acid, which can be further recovered by adopting a suitable method) was evaporated. Add 122g of 1-hydroxyl-3,5-dimethylbenzene, 24g of acetic acid, 122g of tetrachloroethylene, and 102g of concentrated hydrochloric acid to the bottom feed liquid; then install a condenser, a magnetic stirrer, a thermometer, and an oxygen pipe. The reactant was heated to 80°C, and oxygen gas was passed in at a constant speed while stirring. The reaction temperature is controlled between 80-90° C., and the reaction pressure is normal pressure. After the reaction, the lower layer material was separated, and the content was detected by GC; the results are shown in Table 1.

Embodiment 3

[0030] The reaction process is the same as in Example 1, except that acetic acid is replaced with propionic acid respectively. The experimental results are shown in Table 1

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Abstract

The invention provides a 1-hydroxyl-3,5-dimethyl-4-chlorobenzene preparation method, comprising the following steps: adopting 1-hydroxyl-3,5-dimethylbenzene, oxidant and chlorine-containing compound used as chloride source to react in the present of a catalytic system containing cupric salt and lower fatty acid at 0-100 DEG C and at 1-5atm and obtaining the finished product. The reaction can not use other organic solvent or aliphatic chloride as solvent. The method of the invention has simple operation, reaction conditions, high atom economy and selectivity of the prepared target product, little toxic gas in reaction process and less environmental pollution, thus being applicable to large-scale industrialized application.

Description

technical field [0001] The present invention relates to a kind of preparation method of 1-hydroxyl-3,5-dimethyl-4-chlorobenzene, in particular to a kind of under the condition that catalyst and oxidizing agent exist, use chlorine-containing compound to 1-hydroxyl-3,5 -Dimethylbenzene carries out chlorination reaction and prepares the method for 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 d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/28C07C37/62B01J31/30B01J31/04
Inventor 胡汉忠吴飞
Owner 湖南瑞冠生物化工科技有限公司