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Preparation method of high-purity climbazole

A kind of Clambol, high-purity technology, applied in the field of preparation of high-purity Clambol, can solve the problems of high production cost, rising production cost, etc., achieves low production cost, high product quality, and promotes the effect of positive process

Inactive Publication Date: 2017-12-22
江苏绿叶农化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the non-polar solvent used in the recrystallization process of this patent has high production costs, and the final solvent treatment will also cause an increase in production costs.

Method used

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  • Preparation method of high-purity climbazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Dissolve 100kg of chloroetherketone, 30kg of imidazole and 7kg of N,N-dimethylbenzamide in 200kg of toluene, and react at ℃ for 3 hours. After the reaction, add 80 kg of water to wash at 60° C., stand still to separate the water, then cool down to 30° C., crystallize and separate to obtain the crude campanolin. Put 100kg of crude campanola into 200kg of toluene, raise the temperature to 80°C to fully dissolve, add 2kg of activated carbon for press filtration, cool to 30°C to crystallize after press filtration, and then centrifuge to obtain the high-quality clambasu, which is then dried at 65°C. For white crystals. The purity by gas chromatography analysis is 99.92%.

Embodiment 2

[0016] Dissolve 100kg of chloroetherketone, 50kg of imidazole and 10kg of N,N-dimethylbenzamide in 250kg of toluene, and react at 105°C for 4 hours. After the reaction, add 90 kg of water to wash at 55°C, let stand to separate the water, then lower the temperature to 32°C, crystallize and separate to obtain the crude campanolin. Put 100kg of crude campanolin into 270kg of toluene, and heat up to 85°C to fully dissolve. Add 8 mass kg of 30wt.% liquid caustic soda to the toluene to wash, then add 200 mass kg of water to wash, add 3 kg of activated carbon after water separation, press filter, cool to 34 °C to crystallize after press filtration, and then centrifuge to obtain the high-quality clambaosu. Dry the high-quality Campanola at 70°C to obtain white crystals, and the purity is 99.96% by gas chromatography.

Embodiment 3

[0018] Dissolve 100kg of chloroetherketone, 70kg of imidazole and 12kg of N,N-dimethylbenzamide in 300kg of toluene, and react at 105°C for 5 hours. After the reaction, add 100 kg of water to wash at 56°C, let stand to separate the water, then lower the temperature to 35°C, crystallize and separate to obtain crude campanolin. Put 100kg of crude clambasu into 400kg of toluene, raise the temperature to 87°C, fully dissolve, add 3kg of activated carbon for pressure filtration, cool to 35°C to crystallize after press filtration, and then centrifuge to obtain the high-quality climbanol, which is then dried at 73°C , as off-white crystals, the purity of which was analyzed by gas chromatography was 99.91%.

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Abstract

The invention provides a preparation method of high-purity climbazole to prepare the high-purity climbazole. The preparation method comprises the following steps: enabling 200-320 parts of methylbenzene, 100 parts of chloroetherketone, 30-70 parts of imidazole, and 5-12 parts of an acid binding agent by mass to react for 3-5 hours at the temperature of 100-110 DEG C; adding 80-100 parts of water by mass after finishing the reaction, washing with water at the temperature of 50-60 DEG C, standing to divert water, cooling to 30-35 DEG C, crystalizing and separating to obtain a crude product of climbazole; putting 100 parts of crude product of climbazole by mass into 200-400 parts of methylbenzene by mass, raising the temperature to 80-90 DEG C, fully dissolving, adding 1-3 parts of activated carbon by mass, press-filtering, cooling to 30-35 DEG C after press-filtering, crystalizing, centrifuging to obtain a fine product of climbazole, and drying the fine product of the climbazole at the temperature of 65-79 DEG C. The preparation method of the high-purity climbazole has the advantages of simple operation and low production cost.

Description

technical field [0001] The present invention relates to the production method of campanol, in particular, relates to a preparation method of high-purity campanol. Background technique [0002] 1-(4-Chlorophenoxy)-1-(imidazol-1-yl)-3,3-dimethyl-2-butanone, also known as Campanol, has broad-spectrum bactericidal properties and is mainly used to relieve itching and dandruff Conditioning shampoo, hair care shampoo, can also be used in antibacterial soap, shower gel, drug toothpaste, mouthwash and other high-end washing products. Since Campanola is mainly used in daily chemical products, it has strict requirements on color and smell. Pure campanolain is white or off-white crystals. Once the purity is not enough, there will be poor color and odor, which will affect the quality of the final daily chemical products. [0003] "Shanghai Light Industry" 1996 Issue 04, Lu Zuanming, Shen Minqin and Tang Yongjuan's active campanol-a new type of high-efficiency anti-dandruff agent disclo...

Claims

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Application Information

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IPC IPC(8): C07D233/60
CPCC07D233/60
Inventor 乐成芝彭荣贵裴建华陈标
Owner 江苏绿叶农化有限公司
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