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Preparation method of climbazole

A kind of technology of calabasin and toluene, applied in the field of synthetic chemistry, can solve the problems of low efficiency of synthesis, high requirement of reaction conditions, low purity of calabasin, etc., and achieves the effects of reducing production cost, reducing side reactions, and reasonable process design

Inactive Publication Date: 2018-02-27
江苏绿叶农化有限公司
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Problems solved by technology

[0003] In the prior art, there are few synthetic methods for campanol, and the synthesis efficiency is low, the yield is low, and the reaction conditions are high, the environmental protection is poor, and the synthetic campanol has low purity and high cost

Method used

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  • Preparation method of climbazole
  • Preparation method of climbazole
  • Preparation method of climbazole

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0048] Embodiment 1: the preparation method of Campanola, it may further comprise the steps:

[0049] Step 1: Preparation of chloroether ketone

[0050] Preparation of chloropinatone:

[0051] Pump the pinacolone into the pinacolone high-level tank for stand-by; pump methanol into the methanol high-level tank for stand-by;

[0052]The liquid chlorine is vaporized (40°C) from the liquid chlorine cylinder through the vaporizer, and then enters the chlorine gas buffer tank (0.35-0.45MPa), and is controlled by the rotameter. Pass into the chlorination column, open the discharge valves of the pinacolone high-level tank and the methanol high-level tank at the same time, after being mixed by the condenser, pass into the chlorination column to undergo chlorination reaction with the chlorine gas introduced, and the pressure is controlled at about 0.09MPa. The temperature is controlled at -5 to 10°C. The chlorinated pinacolone methanol solution flows into the buffer tank, and then is...

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Abstract

The invention discloses a preparation method of climbazole. According to the method, toluene, chloroetherketone, imidazole and a catalyst, serving as raw materials, react under 100 DEG C to 110 DEG Cfor 4 hours while the temperature is kept, and then the climbazole with the purity being up to 99 percent is prepared by methods, such as crystallization, purification, alkaline wash and recrystallization. Through a lot of experiments, the invention screens out the best climbazole preparation method, the whole process design is reasonable, the process is easy and efficient to operate, in particular, the best reaction conditions screened out, which include catalyst variety, reaction solvent, reaction temperature, reaction time and steps, such as crude reaction of methylbenzene and the climbazole, and alkaline wash thereof, can greatly increase reaction yield (up to 92 percent or above), side reaction is reduced, the reaction rate is increased, the production cost is greatly reduced, and therefore the preparation method of the climbazole has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of synthetic chemistry, and in particular relates to a preparation method of campanolin. Background technique [0002] Campanile, Chinese name: 1-(4-chlorophenoxy)-1-(1H-imidazol-1-yl)-3,3-dimethyl-2-butanone, with broad-spectrum bactericidal properties, mainly It can be used in antipruritic and anti-dandruff conditioning shampoo and hair care shampoo, and can also be used in high-end washing products such as antibacterial soap, shower gel, drug toothpaste, and mouthwash. [0003] In the prior art, there are few synthetic methods for campanol, and the synthesis efficiency is low, the yield is low, and the reaction conditions are high, the environmental protection is poor, and the synthetic campanol has low purity and high cost. Contents of the invention [0004] Purpose of the invention: the purpose of the invention is to overcome the deficiencies in the prior art and provide a method for preparing campan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/60
CPCC07D233/60
Inventor 彭荣贵陈标乐成芝裴建华
Owner 江苏绿叶农化有限公司
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