Refining method of thymol

A technology of thymol and a refining method is applied in the field of medicine and chemical industry, and can solve the problems of impurities such as citronellal and isopulegol, and achieve the effects of improving product purity, simple refining method and reducing refining cost.

Active Publication Date: 2020-01-10
JIANGXI ALPHA HI TECH PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The purpose of the embodiments of the present invention is to provide a method for refining thymol, aiming to solve the problem of citronellal and isopulegol impurities in existing thymol finished products

Method used

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  • Refining method of thymol
  • Refining method of thymol
  • Refining method of thymol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 250g of industrial grade thyme to a 1000ml three-necked flask, add 200ml of n-hexane solvent, pour in nitrogen to replace the air in the reaction flask, under the protection of nitrogen, turn on the stirring, heat up to 70±3℃, keep warm and stir for 0.5 hours to make the thyme brain Fully dissolve and clear; add 2.5g of activated carbon, heat preservation and decolorization for about 1h; filter, the filtrate naturally cools down, slowly stir until granular solids precipitate on the wall of the reaction vessel, adjust the stirring speed, heat preservation and stir quickly for about 1h, and a large amount of crystalline solids ( About 40°C), cool to 5°C, keep stirring and crystallize for 4 hours, filter to obtain 233 g of pure white product, and dry to obtain 214 g of white transparent crystalline powder solid.

Embodiment 2

[0039] Add 250g of industrial grade thyme to a 1000ml three-necked flask, add 250ml of n-heptane solvent, pour in nitrogen to replace the air in the reaction flask, under the protection of nitrogen, turn on stirring, heat up to 75±3℃, keep warm and stir for 0.5 hours to make thyme The brain is fully dissolved; add 5.0g of activated clay, decolorize for about 30min after heat preservation; filter, the filtrate cools naturally, slowly stir until granular solids precipitate on the wall of the reaction vessel, adjust the stirring speed, heat preservation and stir quickly for about 2h, and a large amount of crystals will be precipitated The solid (about 40°C), cooled to 3°C, kept stirring and crystallized for 2 hours, filtered to obtain 231 g of pure white product, and dried to obtain 206 g of white transparent crystalline powder solid.

Embodiment 3

[0041] Add 250g of industrial grade thyme brain to a 1000ml three-necked flask, add 250ml of n-octane solvent, and pass nitrogen to replace the air in the reaction flask. Under the protection of nitrogen, turn on the stirring, heat up to 65±3℃, keep warm and stir for 0.5 hours to make the thyme The brain is fully dissolved; add 2.0g of chromatographic silica gel powder, decolorize after heat preservation for about 1h; filter, the filtrate cools naturally, slowly stir until granular solids precipitate on the wall of the reaction vessel, adjust the stirring speed, heat preservation and stir quickly for about 2h, and a large amount of precipitation The crystalline solid (about 40°C) was cooled to 1°C, kept stirring and crystallized for 6 hours, filtered to obtain 248 g of pure white product, and dried to obtain 186 g of white transparent crystalline powder solid.

[0042] The white transparent crystalline powder solid obtained in Examples 1-3 of the present invention was subjected to...

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Abstract

The invention relates to the technical field of pharmaceutical chemicals, and provides a refining method of thymol. The refining method comprises the steps that a refining solvent is added to crude thymol, and the mixture is heated and stirred sufficiently to obtain a first mixed solution; the amount of the refining solvent is 0.5-3 times the mass-volume ratio of the crude thymol; an adsorbent isadded to the first mixed solution, and thermal insulation decolorization treatment is performed to obtain second mixed liquid; and the second mixed liquid is filtered, the obtained filtrate is subjected to cooling crystallization, thermal insulation crystallization and cooling crystallization separately, then centrifugal filtering is performed, and the thymol is obtained. The refining method can refine impurities such as citronellal and isopulegol in the crude thymol to a hardly detected degree, the purity of the product is effectively improved, and the medical requirements are met; and meanwhile, compared with a traditional rectification method, the refining method is simple, and the refining cost is greatly reduced.

Description

Technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and particularly relates to a refining method of thyme brain. Background technique [0002] Thymol (1963 version of the Chinese Pharmacopoeia), also known as thymol, thymol, and thymol, its chemical name is 2-isopropyl-5-methylphenol. Thymol has a stronger bactericidal effect than phenol and is more toxic Low, has bactericidal and fungicidal effects on the oral and throat mucosa, has antiseptic and local anesthesia effects on the dental caries cavity; can promote the movement of tracheal cilia, is conducive to the secretion of tracheal mucus, is easy to have an expectorant effect, and has a bactericidal effect, so it can be used It is used to treat tracheitis, whooping cough, etc.; it has a strong acaricidal effect, 1% solution has a half-hour mortality rate of 100%, and a 0.03% solution can kill 100% in 24 hours; it can also be used as an ascaris repellent, and it is a versatil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/70C07C37/82C07C37/84C07C39/06
CPCC07C37/685C07C37/70C07C37/82C07C37/84C07C39/06
Inventor 王雪志余志勇缪志毅卢鹏王情英肖青凤
Owner JIANGXI ALPHA HI TECH PHARMA
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