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Preparation method of dihydroartemisinin

A technology of dihydroartemisinin and artemisinin, which is applied in the direction of organic chemistry, can solve the problems of low yield, and achieve the effects of simple preparation method, reduced production cost, and saved solvent

Inactive Publication Date: 2020-03-24
恩施硒禾生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many studies on the synthesis of dihydroartemisinin from artemisinin at home and abroad, but the yield of most of them is about 90%, which is relatively low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] The invention provides a kind of preparation method of dihydroartemisinin, comprising the following steps:

[0021] Artemisinin is first mixed with methanol solution to obtain artemisinin solution;

[0022] The artemisinin solution is mixed with sodium borohydride for a second time to undergo a reduction reaction to obtain dihydroartemisinin;

[0023] The first mixing is carried out under stirring conditions, and the stirring speed of the first mixing is 100r / min;

[0024] The second mixing is carried out under stirring condition, and the stirring speed of the second mixing is 600 r / min.

[0025] In the present invention, unless otherwise specified, the preparation raw materials used are commercially available products well known in the art.

[0026] In the present invention, artemisinin is first mixed with methanol solution to obtain artemisinin solution. In the present invention, the purity of the artemisinin is preferably above 90%; the mass concentration of the m...

Embodiment 1

[0037] Turn on the refrigerating unit, and when the temperature drops to -15°C, stop the refrigerating unit, turn on the refrigerating switch of the reactor, the temperature control switch, and the stirring switch, pour 10L methanol solution (60% in mass concentration) into the reactor, adjust The stirring speed is 100r / min, and 1kg of artemisinin is quickly added;

[0038] Adjust the stirring speed to 600r / min, and when the temperature is 1°C, put 0.35kg of sodium borohydride into it, and carry out the reduction reaction for 1.5h, using ethyl acetate / petroleum ether (volume ratio: 4 / 1) as the developer, and 5% Concentrated sulfuric acid vanillin is used for color development, and whether the reaction is completed by thin-layer chromatography is judged;

[0039] When the reduction reaction reaches the end point, the stirring speed is reduced to 200r / min, and a total of 500mL of acetic acid is added in 3 times. When the temperature is as low as 0°C, the end point is determined ...

Embodiment 2

[0044] Turn on the refrigerating unit, and when the temperature drops to -15°C, stop the refrigerating unit, turn on the refrigerating switch of the reactor, the temperature control switch, the stirring switch, pour 100L methanol solution (60% in mass concentration) into the reactor, adjust The stirring speed is 100r / min, and 10kg of artemisinin is quickly added;

[0045] Adjust the stirring speed to 600r / min, and when the temperature is 1°C, put in 3.1kg of sodium borohydride, and carry out the reduction reaction for 1.8h, using ethyl acetate / petroleum ether (volume ratio: 4 / 1) as the developer, and 5% Concentrated sulfuric acid vanillin is used for color development, and TCL is used to judge whether the reaction is complete;

[0046] When the reduction reaction reaches the end point, the stirring speed is reduced to 200r / min, and a total of 5000mL of acetic acid is added in 3 times. When the temperature is as low as 0°C, the end point is determined by the pH test paper, so tha...

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Abstract

The invention relates to the technical field of organic medicine synthesis, particularly to a preparation method of dihydroartemisinin. According to the invention, sodium borohydride is used as a strong reducing agent to quickly and effectively reduce artemisinin, and a suspension chemical reaction system is established by increasing the stirring speed in a mixing process, so that the heat of thereduction reaction can be quickly dissipated, the reduction reaction speed is increased, the generation of byproducts is effectively inhibited, and the yield and the purity of the product are improved; the preparation method provided by the invention is simple and convenient, saves a large amount of solvents, electricity and heat, shortens the production period and reduces the production cost; andaccording to the embodiments, by adopting the preparation method provided by the invention, the yield of dihydroartemisinin can be up to 110%, and is significantly increased compared with the traditional preparation process, and the preparation method is suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of organic medicine synthesis, in particular to a preparation method of dihydroartemisinin. Background technique [0002] Dihydroartemisinin is an artemisinin derivative with the molecular formula C 15 h 24 o 5 , with a molecular weight of 284.35, is usually used for symptom control of various types of malaria, especially against chloroquine vicious and dangerous malaria; the chemical name is (3R, 5aS, 6R, 8aS, 9R, 12S, 12aR)-eight Hydrogen-3,6,9-trimethyl-3,12-oxo-12H-pyrro[4,3-j]-1,2-benzodisepin 10(3H)alcohol. Dihydroartemisinin is a white needle-like crystal, odorless, bitter in taste, easily soluble in chloroform, soluble in propanol, slightly soluble in methanol or ethanol, almost insoluble in water; melting point is 145-150°C, Decomposes simultaneously when melting. There are many studies on the synthesis of dihydroartemisinin from artemisinin at home and abroad, but the yield of most of them is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20
CPCC07D493/20
Inventor 何美军杨敏
Owner 恩施硒禾生物科技有限公司
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