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Method for recycling mother solution generated in process of producing artemether

A production process, artemether technology, applied in the field of mother liquor recycling, can solve the problems of low yield, no practical value, and many impurities, achieve huge social value and economic value, and improve the overall utilization rate

Active Publication Date: 2012-02-15
浙江来益生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the patent document EP0330520 relates to the process of epimerizing α-arteether into β-arteether, the crystallization yield is 30%-40%, and the yield is relatively low
The patent document CN1106011A converts α-artemether into dihydroartemisinin with a yield of 53%-56%, but repeating the experiment of this patent document did not obtain the dihydroartemisinin claimed in the patent document. The result of long-term reaction is a mixture with more impurities, which has no practical value

Method used

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  • Method for recycling mother solution generated in process of producing artemether
  • Method for recycling mother solution generated in process of producing artemether
  • Method for recycling mother solution generated in process of producing artemether

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Extraction of recyclable substances in artemether mother liquor: 3450ml of mother liquor produced by converting dihydroartemisinin into artemether and washing by rejection filtration was concentrated under reduced pressure at a temperature lower than 40°C in vacuum, and evaporated for about 7 hours. After removing most of the methanol (about 1500ml~2000ml), put ~1350ml of n-heptane into the remaining (1450ml~1950ml) concentrated solution, stir for half an hour, then let stand to separate the water layer (1450ml~1950ml), keep Organic layer 1450ml carries out next step reaction.

[0034]Conversion reaction of recyclable substances: 450ml of n-heptane layer solution, 80ml of methanol and 2.5ml of concentrated HCl were put into a 1000ml four-necked flask, and the reaction was started at a temperature of 30°C. Sampling liquid phase analysis every hour, the content of α-artemether and β-artemether will not change after 8h~12h (α-artemether is 15%~20%, β-artemether is 50%~55% ...

Embodiment 2

[0037] The conversion reaction of recyclable substances: 450ml of n-heptane layer solution, 80ml of methanol and 2.5ml of perchloric acid were put into a 1000ml four-neck flask, and the reaction was started at a temperature of 30°C. Sampling liquid phase analysis every hour, the content of α-artemether and β-artemether will not change after 6h~8h (α-artemether is 12%~16%, β-artemether is 57%~62% %), began to reduce the reaction temperature to 12 ° C ~ 15 ° C.

[0038] Extraction of β-artemether: Add 200ml of about 5% sodium bicarbonate solution to the reaction solution, adjust the pH to neutral, stir for 30min and separate the layers, keep the n-heptane layer for concentration under reduced pressure. Concentrate under vacuum at a temperature of 40°C until it becomes viscous. If it cannot be viscous, it can be entrained with anhydrous methanol until there is basically no organic solvent. For the last concentration, methanol can be used to completely dissolve the viscous matter...

Embodiment 3

[0040] Conversion reaction of recyclable substances: put 450ml of n-heptane layer solution, 80ml of methanol and 2.5ml of concentrated sulfuric acid into a 1000ml four-neck flask, and start the reaction at a temperature of 30°C. Sampling liquid phase analysis every hour, the content of α-artemether and β-artemether will not change after 4h~7h (α-artemether is 12%~18%, β-artemether is 57%~66%) %), began to reduce the reaction temperature to 12 ° C ~ 15 ° C.

[0041] Extraction of β-artemether: Add 200ml of about 5% sodium bicarbonate solution to the reaction solution, adjust the pH to neutral, stir for 30min and separate the layers, keep the n-heptane layer for concentration under reduced pressure. Concentrate under vacuum at a temperature of 40°C until it becomes viscous. If it cannot be viscous, it can be entrained with anhydrous methanol until there is basically no organic solvent. For the last concentration, methanol can be used to completely dissolve the viscous matter an...

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Abstract

The invention provides a method for recycling mother solution generated in the process of producing artemether. In the conventional method for recycling alpha-artemether, the integral utilization rate of unit artemisinin and the total yield of beta-artemether are low. The method comprises the following steps of: evaporating artemether mother solution generated in the process of producing the artemether to remove methanol, performing concentration pretreatment, extracting by using a solvent, converting part of alpha-artemether and dihydroartemisinin into the beta-artemether in the presence of acid serving as a catalyst, neutralizing, washing, concentrating, and recrystallizing in a methanol-water system to generate the beta-artemether with high purity. The process is simple and high in recycling value and can be used for industrial production.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a method for recycling mother liquor produced in the production process of artemether. Background technique [0002] Artemisinin is a sesquiterpene lactone compound with a peroxide bridge structure extracted and isolated from the leaves of Artemisia annua by Chinese pharmaceutical workers in 1971. It is the first successfully developed in my country in the world. A new antimalarial drug. On the basis of artemisinin, through structural modification, derivatives such as artemether, artether, and artesunate are obtained. The antimalarial activity of artemether is 6 times that of artemisinin. [0003] Artemether is obtained from dihydroartemisinin by reduction of artemisinin first, and then by etherification. Artemisinin is generally extracted from Artemisia annua, and Artemisia annua generally contains about 0.7% of artemisinin, which is very low. Artemether has two epimers, α-ar...

Claims

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Application Information

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IPC IPC(8): C07D493/20
CPCY02P20/582
Inventor 俞永浩贺文彪马秀英曹瑞伟杨建峰
Owner 浙江来益生物技术有限公司
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