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Crystallization method for preparing high-purity idebenone

A technology for crystallization of idebenone, which is applied in the field of compound separation and purification, can solve the problems of low purity and low yield of idebenone, and achieve the effects of high purity and yield, simple operation and strong controllability

Inactive Publication Date: 2012-03-28
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to overcome the problems of low purity and low yield of idebenone products caused by the existing crystallization process, and provide a new method for crystallization and purification of idebenone

Method used

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  • Crystallization method for preparing high-purity idebenone
  • Crystallization method for preparing high-purity idebenone
  • Crystallization method for preparing high-purity idebenone

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Weigh 1.0 g of crude idebenone into a 200 mL jacketed glass crystallizer, measure 5 mL of dichloromethane with a graduated cylinder, and add it into the crystallizer at room temperature to completely dissolve idebenone. The temperature inside the crystallizer was controlled by a Julabo F32 refrigeration / heating circulating water bath, and the stirring was carried out by a Corning PC-353 magnetic stirrer. Then 35 mL of n-hexane was added to the crystallizer at room temperature, and the clear solution became cloudy. Heating the solution temperature to 36°C, the cloudy solution became clear. Filter the clarified liquid while it is hot, and place the filtrate in another 200 mL crystallizer. At this time, the temperature of the solution drops slightly, and then continue to heat to 36°C, keep the temperature constant for 30 minutes, and cool down to 0°C at a rate of 0.1°C / min. . As the temperature decreased, idebenone crystals slowly precipitated, filtered and washed (w...

Embodiment 2

[0036](1) Weigh 1.2 g of crude idebenone into a 200 mL jacketed glass crystallizer, measure 6 mL of dichloromethane with a graduated cylinder, and add it into the crystallizer at room temperature to completely dissolve idebenone. The temperature inside the crystallizer was controlled by a Julabo F32 refrigeration / heating circulating water bath, and the stirring was carried out by a Corning PC-353 magnetic stirrer. Then 42 mL of n-hexane was added to the crystallizer at room temperature, and the clear solution became cloudy. Heating the solution temperature to 36°C, the cloudy solution became clear. Filter the clarified liquid while it is hot, and place the filtrate in another 200 mL crystallizer. At this time, the temperature of the solution drops slightly, and then continue to heat to 36°C, keep the temperature constant for 30 minutes, and cool down to 0°C at a rate of 0.1°C / min. . As the temperature decreased, idebenone crystals slowly precipitated, filtered and washed (wa...

Embodiment 3

[0039] (1) Weigh 1.6 g of crude idebenone into a 200 mL jacketed glass crystallizer, measure 8 mL of dichloromethane with a graduated cylinder, and add it into the crystallizer at room temperature to completely dissolve idebenone. The temperature inside the crystallizer was controlled by a Julabo F32 refrigeration / heating circulating water bath, and the stirring was carried out by a Corning PC-353 magnetic stirrer. Then 56 mL of n-hexane was added to the crystallizer at room temperature, and the clear solution became cloudy. Heating the solution temperature to 36°C, the cloudy solution became clear. Filter the clarified liquid while it is hot, and place the filtrate in another 200 mL crystallizer. At this time, the temperature of the solution drops slightly, and then continue to heat to 36°C, keep the temperature constant for 30 minutes, and cool down to 0°C at a rate of 0.1°C / min. . As the temperature decreased, idebenone crystals slowly precipitated, filtered and washed (w...

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Abstract

The utility model relates to a crystallization method for preparing high-purity idebenone, belonging to the technical field of compound separation and purification. The crystallization method includes the steps as follows: firstly, dissolving crude idebenone in big-polarity good solvent dichloromethane, thus obtaining clear solution; adding a certain amount of small-polarity antisolvent normal hexane in the clear solution, thus making the solution to become turbid; increasing temperature until the burbid solution becomes clear; cooling the clear solution by slowing reducing the temperature; and crystallizing the idebenone product out from the solvent and leaving impurities in mother solution. In the invention, a two-step method of antisolvent crystallization and cooling crystallization is adopted and the phenomenon of oil separation is avoided by controlling the types and the proportioning of mixed solvent as well as the crystallization starting concentration, the temperature and the cooling rate. The invention firstly discloses a new crystallization method for purifying idebenone by controlling oil separation; by the adoption of the method, the crystallization product of the idebenone is up to above 99.5% in purity and above 78% in yield.

Description

technical field [0001] The invention relates to a method for separating and purifying the drug idebenone, more specifically, the invention relates to a new crystallization method for preparing high-purity idebenone. The invention belongs to the technical field of compound separation and purification. Background technique [0002] Idebenone is a new anti-senile dementia special drug, brain function metabolism and mental symptom improvement drug. In recent years, this product has been widely used in cosmetics and food industries, and it mainly plays an anti-oxidation role. It is one of the most effective external antioxidants. However, chemically synthesized idebenone products generally contain about 1% to 2% of unknown impurities. As people's requirements for impurities become more and more stringent, if the impurities are not separated from the product, the efficacy of the drug will be affected , and even affect human health. Therefore, reducing the impurity content as mu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/28C07C46/10
Inventor 陆杰李义平李祯汪晶舒亮
Owner JIANGNAN UNIV
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