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Method for preparing dihydroartemisinin crude drug by single process

A technology of dihydroartemisinin and raw materials, which is applied in the fields of resisting vector-borne diseases and organic chemistry, etc., can solve the problem that the raw materials of dihydroartemisinin cannot be produced, cannot meet the environmental requirements of raw materials, and cannot achieve dust-free Aseptic operation and other issues, to achieve the effect of reducing the difficulty of recycling, reducing the amount of use, and reducing the difficulty of separation

Inactive Publication Date: 2019-07-23
ZHANG JIA GANG VINSCE BIO PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, in this production process, the crystals are obtained by vacuum filtration after neutralization, and then the crystals are washed with aqueous methanol solution. The above two steps can only be completed in a common experimental environment, and dust-free and sterile operations cannot be realized (dust in the control environment , microorganisms and other parameters), that is, it cannot meet the environmental requirements stipulated in the production of raw materials
[0008] Therefore, this production process can only be used for the preparation of intermediates of dihydroartemisinin, but cannot be used for the production of dihydroartemisinin raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] A method for preparing a dihydroartemisinin bulk drug in a single flow process, comprising the steps of:

[0048] S1. Dissolving 100kg artemisinin in 600L toluene;

[0049] S2. Add 50L of an aqueous solution containing 0.5kg of benzyltriethylammonium chloride, cool down to -10°C, and start adding sodium borohydride reducing agent in batches under nitrogen protection, totaling 16kg, and control the temperature not to exceed 0°C. Continue to react for 5 hours, monitor with thin-layer chromatography, when the artemisinin spots disappear completely, the reaction is considered complete;

[0050] S3. Regulate the pH value of the reaction system obtained in step S2 to 7 with a mass concentration of 25% acetic acid solution, and control the temperature of the system during the adjustment process to be 0-5°C; this process is completed in an automatic interlock device, and the automatic interlock The device includes a temperature sensor, a pH sensor, a sampling controller, a sti...

Embodiment 2

[0055] A method for preparing a dihydroartemisinin bulk drug in a single flow process, comprising the steps of:

[0056] S1. Dissolving 100kg artemisinin in 600L dichloromethane;

[0057] S2. Add 50L of an aqueous solution containing 0.5kg of benzyltriethylammonium chloride, cool down to -10°C, and start adding sodium borohydride reducing agent in batches under nitrogen protection, totaling 16kg, and control the temperature not to exceed 0°C. Continue to react for 5 hours, monitor with thin-layer chromatography, when the artemisinin spots disappear completely, the reaction is considered complete;

[0058] S3. Adjust the pH value of the reaction system obtained in step S2 to 7 with a mass concentration of 25% acetic acid solution, and control the temperature of the system during the adjustment process to be 0-5 ° C; the above operation is completed using the same automatic interlocking device as in Example 1; add water After stirring, separate the liquids, extract the aqueous ...

Embodiment 3

[0062] A method for preparing a dihydroartemisinin bulk drug in a single flow process, comprising the steps of:

[0063] S1. Dissolving 100kg artemisinin in 600L toluene;

[0064] S2. Add 50L of an aqueous solution containing 0.5kg of benzyltriethylammonium chloride, cool down to -10°C, and start adding sodium borohydride reducing agent in batches under nitrogen protection, totaling 16kg, and control the temperature not to exceed 0°C. Continue to react for 5 hours, monitor with thin-layer chromatography, when the artemisinin spots disappear completely, the reaction is considered complete;

[0065] S3. Adjust the pH value of the reaction system obtained in step S2 to 7 with a mass concentration of 25% acetic acid solution, and control the temperature of the system during the adjustment process to be 30° C.; the above operation is completed with the automatic interlocking device in Example 1; after adding water and stirring Separating the liquid, extracting the aqueous phase ob...

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Abstract

The invention belongs to the technical field of production of dihydroartemisinin crude drugs, and particularly relates to a method for preparing a dihydroartemisinin crude drug through a single process. The method comprises the following steps: S1, dissolving artemisinin in a non-protonic solvent; S2, sequentially adding a phase transfer catalyst and a reducing agent, and performing reduction reaction on the artemisinin; S3, adjusting the pH value of the reaction system obtained in step the S2 to 5-7 with acid liquor, adding water, stirring, performing liquid separating, extracting a water phase obtained by the liquid separating with the same non-protonic solvent as in the step S1, and finally combining an organic phase obtained by the extracting with an organic phase obtained by liquid separating, washing with water, and drying; and S4, precipitating crystals from the dried organic phase obtained by the S3 in a crystallization-filter pressing-drying three-in-one crystallization device, then concentrating, filter-pressing and drying to obtain a dihydroartemisinin refined product. The invention provides the method for preparing the high-purity dihydroartemisinin crude drug, and thepurity and the yield of the dihydroartemisinin prepared by the method can reach more than 99%.

Description

technical field [0001] The invention belongs to the technical field of production of dihydroartemisinin raw materials, in particular to a method for preparing dihydroartemisinin raw materials in a single process. Background technique [0002] Dihydroartemisinin (Dihydroartemisinin) is an artemisinin derivative, the chemical name is (3R, 5aS, 6R, 8aS, 9R, 12S, 12aR)-octahydro-3,6,9-trimethyl-3 , 12-oxo-12H-pyridine[4,3-j]-1,2-benzodioxane-10(3H)-ol. Molecular formula is C 15 h 24 o 5 , the molecular weight is 284.35. Dihydroartemisinin is white needle crystal; odorless, bitter taste. Soluble in chloroform, soluble in propanol, slightly soluble in methanol or ethanol, almost insoluble in water. The melting point of dihydroartemisinin is 145-150°C, and it decomposes when melting. Dihydroartemisinin is the active metabolite of artemisinin drugs. Experimental results show that dihydroartemisinin has pharmacological effects such as antimalarial, antitumor, antiviral, and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20
CPCC07D493/20Y02A50/30
Inventor 彭学东张梅赵金召闫勇义
Owner ZHANG JIA GANG VINSCE BIO PHARM
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