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Method for preparing artemether from artemether synthetic mother liquor

A technology for synthesizing mother liquor and artemether, which is applied in organic chemistry and other fields, can solve the problems of complex regeneration of silica gel, high production cost, and difficulty in popularization and application, and achieve the effects of low production cost, easy recycling, and simple and easy-to-control process operation

Inactive Publication Date: 2013-02-06
GUILIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above method can separate α-artemether, it adopts silica gel column for separation, adopts complex eluent, has the disadvantages of high production cost and complex regeneration of silica gel, and is difficult to be popularized and applied in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Weigh 5 grams of raw materials, dissolve them with 15ml of acetone, and put them on a D101 type macroporous resin column, elute with 40% acetone (flow rate is 6ml / min), detect by thin-layer chromatography, and collect α-artemisia in sections. The eluate of ether and the eluate containing β-artemether, the acetone in the above-mentioned eluate containing α-artemether was recovered under reduced pressure, and filtered to obtain 1.5 g of crude α-artemether; recovery under reduced pressure The acetone in the above-mentioned eluent containing β-artemether was filtered to obtain 2.5 grams of β-artemether crude product;

[0023] 2) α-artemether crude product and β-artemether crude product are respectively dissolved in ethanol equivalent to 3.3 times of their respective weights at 40°C, and water equivalent to 3 times of their respective weights is added dropwise after dissolving. , cooled to 12 ° C and stirred for 30 minutes, a large number of white crystals were precipitat...

Embodiment 2

[0026] 1) Weigh 5 grams of raw materials, dissolve with 15ml of acetone, and put on a D102 type macroporous resin column, elute with 60% acetone (flow rate is 5ml / min), detect by thin-layer chromatography, and collect α-artemisia in sections. The eluate of ether and the eluate containing β-artemether, the acetone in the above-mentioned eluate containing α-artemether was recovered under reduced pressure, and filtered to obtain 1.8 g of crude α-artemether; recovery under reduced pressure The acetone in the above-mentioned eluent containing β-artemether was filtered to obtain 2.2 grams of β-artemether crude product;

[0027] 2) α-artemether crude product and β-artemether crude product are respectively dissolved in ethanol equivalent to 4 times of their respective weights at 40°C, and water equivalent to 3 times of their respective weights is added dropwise after dissolving. , cooled to 10 ℃ and stirred for 20 minutes, a large number of white crystals were precipitated, suction fi...

Embodiment 3

[0030] 1) Weigh 10 grams of raw materials, dissolve them with 30 ml of methanol, and put them on an AB-8 macroporous resin column, elute with 50% acetone (flow rate is 6 ml / min), detect by thin-layer chromatography, and collect α- The eluate of artemether and the eluate containing β-artemether, the acetone in the above-mentioned eluate containing α-artemether was recovered under reduced pressure, and filtered to obtain 4 grams of crude α-artemether; The acetone in the above-mentioned eluent containing β-artemether was recovered under pressure, and filtered to obtain 5 grams of β-artemether crude product;

[0031] 2) α-artemether crude product and β-artemether crude product are respectively dissolved in ethanol equivalent to 5 times of their respective weights at 40°C, and water equivalent to 4 times of their respective weights is added dropwise after dissolving. , cooled to 12 ℃ and stirred for 130 minutes, a large number of white crystals were precipitated, suction filtration...

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Abstract

The invention discloses a method for preparing artemether from artemether synthetic mother liquor. The method includes: using organic solvent to dissolve solid obtained by concentrating and drying artemether synthetic mother liquor, sampling on a macroporous resin column, using acetone with the volume concentration of 20-70% for eluting, performing thin layer chromatographic detection, and fractionally collecting eluant containing alpha-artemether and eluant containing beta-artemether; and respectively recovering solvents in the eluant containing alpha-artemether and the eluant containing beta-artemether, filtering to obtain crude alpha-artemether and crude beta-artemether, using ethanol to dissolve the crude alpha-artemether and the crude beta-artemether, and adding water for crystallization to obtain alpha-artemether and beta-artemether. Compared with the prior art, the method has the advantages that the alpha-artemether and the beta-artemether are successively separated from the artemether synthetic mother liquor, filler for chromatography is cheap and simple in regeneration, and elution solvent is simple and easy to recovery; and the whole process is simple and easy to control, the production cost is low, and industrial production is easier to implement.

Description

technical field [0001] The invention relates to a preparation method of artemether, in particular to a method for preparing artemether from artemether synthesis mother liquor. Background technique [0002] Artemether (methyldihydroartemisinine, MDA) is a methyl etherified derivative of dihydroartemisinin. It is a derivative of artemisinin, a sesquiterpene lactone, obtained after semi-synthesis of artemisinin extracted from the plant Artemisia annua , its epimer β-artemether is the first-choice antimalarial drug recommended by the World Health Organization, and is a new type of drug developed by my country and recognized internationally. Artemether is more effective than artemisinin in treating multidrug-resistant and complicated strains of Plasmodium falciparum. However, about 20% of the α isomer, α-artemether, is generated during the preparation process of artemether. α-artemether has no antimalarial effect and is only used as a standard in the detection of β-artemether. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20
Inventor 郑清四袁胜雄
Owner GUILIN PHARMA
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