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Method for extracting and purifying dihydroartemisinic acid from artemisinin wax oil

A technology for purifying dihydroartemisinic acid and artemisinin, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as underutilization of dihydroartemisinic acid

Inactive Publication Date: 2014-04-02
湘西自治州奥瑞克医药化工有限责任公司 +1
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AI Technical Summary

Problems solved by technology

However, in the existing production process, although dihydroartemisinic acid is extracted, it is treated as waste after being mixed with a large amount of wax oil during column chromatography elution and crystallization, and the dihydroartemisinic acid in it is not fully recovered. use

Method used

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Examples

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Effect test

example 1

[0019] Take 500 kilograms of wax oil from the artemisinin production process, add 2500L of 2% (M / V) sodium bicarbonate aqueous solution, heat to 75°C, stir for 2 hours, then add an appropriate amount of saturated sodium bicarbonate aqueous solution to adjust the pH to 9. Stir for another 30 minutes. After cooling, centrifuge to obtain 2350L of centrifugal fluid. 600L of petroleum ether was added to the centrifugal liquid for extraction and degreasing twice. The degreasing water phase was heated and evaporated to remove the remaining small amount of petroleum ether, then diluted hydrochloric acid was added to adjust the PH value to 5-6, let it cool to room temperature to crystallize for 12 hours, and suction filtered to obtain 31 kg of crude crystals. The crude crystals were dissolved in an appropriate amount of ethyl acetate and then crystallized to obtain 23 kilograms of crystalline product, with a content of 98.6% detected by HPLC.

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Abstract

The invention discloses a method for extracting and purifying dihydroartemisinic acid from artemisinin wax oil. The method comprises the following steps: adding wax oil into a sodium hydrogen carbonate water solution, heating, adjusting the pH value to be 9-9.5 by the saturated sodium hydrogen carbonate water solution after the wax oil is completely molten, stirring and conducting a centrifuging process; adding petroleum ether into centrifugal liquid, stirring, extracting and degreasing; heating a degreased alkali water solution to remove residual petroleum ether, adding hydrochloric acid for adjusting the pH value to be 5-6, naturally cooling to room temperature, and crystallizing; dissolving crystals by ethyl acetate, and re-crystallizing to obtain dihydroartemisinic acid. According to the method, waste wax oil can be effectively utilized and the yield of dihydroartemisinic acid can be increased.

Description

Technical field [0001] The invention relates to a method for extracting and purifying artemisinin biosynthetic precursors from artemisinin wax oil, in particular to a method for extracting and purifying dihydroartemisinic acid from artemisinin wax oil. Background technique [0002] Arteannuin is an anti-malarial active ingredient extracted from the traditional Chinese medicine Artemisa annua, which has anti-leukemia and immune regulation functions. [0003] At present, artemisinin is mainly extracted from Artemisia annua. In addition to artemisinin, Artemisia annua also contains other sesquiterpenoids, such as artemisinin G, artemisinin A, artemisinin B, artemisinin C, artemisinin, artemisinin, Table deoxy artemisinin, artemisinol, methyl artemisinate, artemisinic acid, 6,7-dehydroartemisinic acid, dihydroartemisinic acid, etc. Among them, artemisinic acid and dihydroartemisinic acid have the highest content and utilization value. [0004] Dihydroartemisinic acid is an intermediat...

Claims

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Application Information

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IPC IPC(8): C07C57/26C07C51/487
CPCC07C51/487C07C57/26
Inventor 胡灿华张慧云
Owner 湘西自治州奥瑞克医药化工有限责任公司
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