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Preparing method for 4-chlorine-3,5-xylenol

A technology of dimethylphenol and divalent copper, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems such as the reduction of PCMX yield, and achieve the effect of high total conversion rate and good selectivity.

Active Publication Date: 2014-12-31
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

[0011] Due to the existence of dimerization reaction, the yield of PCMX is greatly reduced

Method used

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  • Preparing method for 4-chlorine-3,5-xylenol
  • Preparing method for 4-chlorine-3,5-xylenol
  • Preparing method for 4-chlorine-3,5-xylenol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 1222g (10mol) 3,5-dimethylphenol, 244.4g copper chloride dihydrate, and 861g concentrated hydrochloric acid (HCl8.5mol) respectively in the 5000m1 three-necked reaction flask; then install a condenser, magnetic stirring, thermometer, and Oxygen tube. The reactant was heated to 90°C, and oxygen gas was passed in at a constant speed while stirring. The reaction temperature is controlled at 90°C, the reaction pressure is normal pressure, and the conversion rate is monitored by sampling in the middle of the reaction. The reaction ends when the reaction conversion rate reaches about 85%. After the reaction, the upper organic phase was taken to detect the content by HPLC (see Table 1). The upper organic phase was rectified, and the former fraction (3,5-dimethylphenol) (content 98%) was recovered, and the content of the obtained product was detected by HPLC (see Table 2).

Embodiment 2

[0034]Add 1222g (10mol) 3,5-dimethylphenol, 244.4g copper chloride dihydrate (CuCl 2 1.43mol), and 861g concentrated hydrochloric acid (HCl8.5mol); then install a condenser, magnetic stirring, thermometer, and oxygen tube. The reactant was heated to 95°C, and oxygen gas was passed in at a constant speed while stirring. The reaction temperature is controlled at 95°C, the reaction pressure is normal pressure, the conversion rate is monitored by sampling during the reaction, and the conversion rate is controlled at about 85%. After the reaction, the upper organic phase was taken to detect the content by HPLC (see Table 1). The upper organic phase was rectified, and the unreacted front fraction 3,5-dimethylphenol (content 98.1%) was recovered, recrystallized and washed to obtain the target product, and the content was detected by HPLC (see Table 2).

Embodiment 3

[0036] Add 1222g (10mol) 3,5-dimethylphenol, 244.4g copper chloride dihydrate (CuCl 2 1.43mol), and 861g concentrated hydrochloric acid (HCl8.5mol); then install a condenser, magnetic stirring, thermometer, and oxygen tube. The reactant was heated to 98°C, and oxygen gas was passed in at a constant speed while stirring. The reaction temperature is controlled at 98°C, the reaction pressure is normal pressure, the conversion rate is monitored by sampling during the reaction, and the conversion rate is controlled at about 85%. After the reaction, the upper organic phase was taken to detect the content by HPLC (see Table 1). The upper organic phase was rectified to recover the unreacted 3,5-dimethylphenol (content 98.3%), recrystallized and washed to obtain the target product, and the content was detected by HPLC (see Table 2).

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Abstract

The invention provides a preparing method for 4-chlorine-3,5-xylenol. Cupric salt taken as catalyst reacts with 3,5-xylenol, oxygen and hydrochloric acid in inorganic and organic solvent, so as to obtain the 4-chlorine-3,5-xylenol. In order to further optimize the reaction process, the reaction is terminated when the conversion rate of the raw material, namely the 3,5-xylenol, reaches 50-90%, so that the generation of bipolymer is avoided, the selectivity of a target product is excellent, the total conversion rate is higher, the report method for preparing 4-chlorine-3,5-xylenol through oxidization and chlorination is completely optimized, as a result, the preparation of 4-chlorine-3,5-xylenol through oxidization and chlorination is completely suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of 4-chloro-3,5-dimethylphenol. When divalent copper salt is used as a catalyst to prepare the target product by reacting with 3,5-dimethylphenol, oxygen and hydrochloric acid, by controlling the conversion rate of 3,5-dimethylphenol to avoid the generation of dimer by-products , improve the total yield of 4-chloro-3,5-dimethylphenol, and make it economical for industrial production. Background technique [0002] 4-Chloro-3,5-dimethylphenol (also known as: p-chloro-m-dimethylphenol, CAS number: 88-04-0, English abbreviation: PCMX) is an important microbial killer, as an antibacterial Agent, antifungal agent, disinfectant, widely used in industry and cosmetic industry, it has excellent inhibitory effect on bacteria, mold and most fungi. In recent years, with the ravages of epidemic diseases, people's health awareness has become stronger and stronger. As a traditional low-toxicity disinfectant, 4-chloro-3,5...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/62C07C39/28
Inventor 吴飞胡汉忠张新波李培俊
Owner 湖南瑞冠生物化工科技有限公司
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