Preparation process of artemether

A preparation process, technology of artemether, applied in the field of preparation of high-purity β-artemether, can solve the problems of low content of β-artemether, complex operation, etc., to achieve recycling, short production cycle, and energy saving Effect

Inactive Publication Date: 2014-02-12
CHONGQING HOLLEY PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is complicated to operate and requires freezing reaction, and the content of β-artemether in the obtained product is still not high

Method used

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  • Preparation process of artemether

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh 100g of dihydroartemisinin, put it into a 2000ml three-necked bottle, and add 1000ml of dimethyl carbonate and 5ml of boron trifluoride methyl ether successively under stirring. React at room temperature for 2 hours, take a sample for thin-layer chromatography (TLC) to detect no dihydroartemisinin spots, that is, dihydroartemisinin has completely reacted. The pH of the solution was adjusted to 7 by adding saturated sodium bicarbonate solution. The reaction solution was concentrated to dryness at 50°C under vacuum to obtain 98.23 g of artemether crude crystals. Artemether coarse crystals were dissolved in methanol, crystallized at low temperature, and dried at 50°C to obtain the artemether product, which contained 95.16 g of β-artemether through detection and calculation.

Embodiment 2

[0031] Weigh 100g of dihydroartemisinin, put it into a 2000ml three-necked bottle, and add 1500ml of dimethyl carbonate and 5ml of boron trifluoride methyl ether successively under stirring. React at room temperature for 2 hours, and take a sample TLC to detect no dihydroartemisinin spots. The pH of the solution was adjusted to 7 by adding saturated sodium bicarbonate solution. The reaction solution was concentrated to dryness at 50°C under vacuum to obtain 98.46 g of artemether crude crystals. Artemether coarse crystals were dissolved in methanol, crystallized at low temperature, and dried at 50°C to obtain the artemether product, which contained 95.32 g of β-artemether through detection and calculation.

Embodiment 3

[0033] Weigh 100g of dihydroartemisinin, put it into a 2000ml three-necked bottle, and add 1000ml of ethyl acetate and 10ml of boron trifluoride methyl ether successively under stirring. After reacting at room temperature for 1.5 hours, no dihydroartemisinin spots were detected by sampling TLC. The pH of the solution was adjusted to 7 by adding saturated sodium bicarbonate solution. The reaction solution was concentrated to dryness at 50°C under vacuum to obtain 98.36 g of artemether crude crystals. Artemether coarse crystals were dissolved in methanol, crystallized at low temperature, and dried at 50°C to obtain the artemether product, which contained 95.25 g of β-artemether through detection and calculation.

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Abstract

The invention relates to a process for preparing high-purity beta-artemether, and aims to provide a preparation process of artemether, and the preparation process has the advantages of easiness in technological operation, low cost and high yield. The preparation process of the artemether comprises the following steps: a, etherifying, namely adding dihydroartemisinin into an ester solvent to perform etherification reaction under the action of a catalyst; b, concentrating, namely concentrating and drying the etherification product to obtain the product. The preparation process is simple and easy to operate and is suitable for industrialization; the reaction solvent and an etherifying agent in the entire process are the same solvent, namely the ester solvent, so that the control over the industrial production is more facilitated, and the recovery and reuse of the solvent are also facilitated; the yield of the beta-artemether in the prepared product reaches over 95 percent, the raw material is greatly saved, and the production cost is reduced; the time of the entire synthesis reaction is only 1-2 hours, so that the production period is short; the reaction can be excellently performed under the room temperature condition without freezing treatment, so that energy is saved, and industrial production is also facilitated.

Description

technical field [0001] The invention relates to a process for preparing artemether, in particular to a process for preparing high-purity β-artemether. Background technique [0002] Artemisinin is a sesquiterpene lactone drug with peroxy groups extracted from the traditional Chinese medicine Artemisia annua, and it is a specific drug for the treatment of malaria caused by Plasmodium falciparum. Derivatives of artemisinin mainly include artesunate, artemether and dihydroartemisinin. [0003] Artemether (English name Artemether), also known as methyl hydrogen-reduced artemisinin or artemisinin methyl ether, is odorless, slightly bitter, easily soluble in acetone or chloroform, and easily soluble in ethanol or ethyl acetate. Almost insoluble in water, with a melting point of 86-90°C. Artemether is a specific drug independently developed by China for the treatment of various critically ill malaria patients and the rescue of cerebral malaria patients. It has fast drug effect, go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20
CPCC07D493/20
Inventor 刘永源罗晓江欧阳敏杨再辉黄元军刘晓东
Owner CHONGQING HOLLEY PHARMA
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