Method for preparing high-purity dihydroartemisinic acid by removing grease from crude dihydroartemisinic acid

A high-purity technology of dihydroartemisinic acid, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems affecting the purity of dihydroartemisinic acid, high oil impurities, etc., and achieves easy industrialization and promotion, The effect of removing grease impurities and reducing production costs

Active Publication Date: 2019-08-20
HUNAN AGRICULTURAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the actual production process of preparing dihydroartemisinic acid from artemisinin waste oil, the crude product of

Method used

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  • Method for preparing high-purity dihydroartemisinic acid by removing grease from crude dihydroartemisinic acid
  • Method for preparing high-purity dihydroartemisinic acid by removing grease from crude dihydroartemisinic acid
  • Method for preparing high-purity dihydroartemisinic acid by removing grease from crude dihydroartemisinic acid

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Experimental program
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Embodiment 1

[0040] A method for preparing high-purity dihydroartemisinic acid by removing oil from crude dihydroartemisinic acid, comprising the following steps:

[0041](1) Primary crystallization: using 100 g of crude dihydroartemisinic acid with a content of 30.0% as a raw material, add 10 ml of methanol with a volume concentration of 50%, stir for 0.5 h, and stand for 48 h to crystallize;

[0042] (2) Centrifugal deoiling: centrifuge after the crystalline liquid crystallization in step (1) is complete, the filter cloth mesh number during described centrifugation is 100 orders, and the rotating speed is 700r / min, and centrifugation time is 4h, obtains off-white crystal and grease, The oil was repeated 4 times according to step (1), and combined to obtain 37.1 g of off-white crystals; the content of dihydroartemisinic acid in the obtained off-white crystals was 73% as detected by HPLC;

[0043] (3) Dissolving and deoiling: Add 742ml of methanol with a volume concentration of 50% to the ...

Embodiment 2

[0049] A method for preparing high-purity dihydroartemisinic acid by removing oil from crude dihydroartemisinic acid, comprising the following steps:

[0050] (1) Primary crystallization: 10 kg of crude dihydroartemisinic acid with a content of 32.5% was used as raw material, 5 L of n-butanol with a volume concentration of 60% was added, stirred for 1 hour, and left to stand for 24 hours to crystallize;

[0051] (2) Centrifugal deoiling: centrifuging after the crystalline liquid crystallization in step (1) is complete, the filter cloth mesh number during described centrifugation is 200 orders, and the rotating speed is 1400r / min, and centrifugation time is 3h, obtains off-white crystallization and grease, The fats and oils were repeated twice according to step (1), and 3.65 kg of off-white crystals were obtained by merging; the content of dihydroartemisinic acid in the obtained off-white crystals was 78% as detected by HPLC;

[0052] (3) Dissolving and deoiling: Add 54.75 L of...

Embodiment 3

[0058] A method for preparing high-purity dihydroartemisinic acid by removing oil from crude dihydroartemisinic acid, comprising the following steps:

[0059] (1) Primary crystallization: take 1000 kg of crude dihydroartemisinic acid with a content of 31.2% as raw material, add 1000 L of a mixture of ethyl acetate and industrial hexane with a volume concentration of 70% and a volume ratio of 2:1, and stir for 1.5 h , standing for 72h to crystallize;

[0060] (2) Centrifugal deoiling: centrifuge after the crystalline liquid crystallization in step (1) is complete, the filter cloth mesh number during described centrifugation is 400 orders, and the rotating speed is 2100r / min, and centrifugation time is 2h, obtains off-white crystal and grease, The fats and oils were repeated once according to step (1) to obtain 365.9 kg of off-white crystals; the content of dihydroartemisinic acid in the obtained off-white crystals was 81.2% as detected by HPLC;

[0061] (3) Dissolving and deoi...

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Abstract

The invention relates to the field of medicinal chemistry, in particular to a method for preparing high-purity dihydroartemisinic acid by removing grease from crude dihydroartemisinic acid. The methodof the invention comprises the following steps: (1) preliminary crystallization; (2) centrifugal degreasing; (3) dissolving for degreasing; (4) recrystallization; (5) decolorization and crystallization; (6) secondary decolorization and recrystallization; (7) drying; and (8) pulverizing and packaging. The method of the invention uses the crude dihydroartemisinic acid as a raw material, and can remove most of grease impurities in the crude dihydroartemisinic acid and prepare high-purity dihydroartemisinic acid through centrifugation via a centrifuge, solution extraction and multiple dissolutiondegreasing and crystallization. The method of the invention is simple to operate, capable of effectively removing grease impurities in the crude dihydroartemisinic acid, and easy to be industrializedand popularized; and the finally prepared dihydroartemisinic acid has a content of 99% or more and a purity of 99.9%, and can meet the needs of chemical synthesis, pharmaceutical preparation and thelike.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a method for preparing high-purity dihydroartemisinic acid by removing oil from crude dihydroartemisinic acid. Background technique [0002] Artemisinin is a new type of antimalarial drug discovered by Mr. Tu Youyou, a famous Chinese pharmacist and winner of the 2015 Nobel Prize in Medicine, which has the advantages of "high efficiency, quick action, and low toxicity". It has special effects. From 1973 when artemisinin was discovered to 2018, in the past few decades, artemisinin and artemisinin derivatives have developed into a large industry with an annual output value of 1.5 billion US dollars, and the price of artemisinin In 2012, the price peaked at 5,800 yuan per kilogram in recent years and then fell all the way to 950 yuan per kilogram in 2016. From 2016 to 2018, the price of artemisinin has been at 950-1200 yuan per kilogram for two years. The price range of artemisini...

Claims

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Application Information

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IPC IPC(8): C07C51/43C07C57/26
CPCC07C51/43C07C2602/28C07C57/26
Inventor 彭国平廖书桥欧阳斌
Owner HUNAN AGRICULTURAL UNIV
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