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Method for preparing indirubin

A technology of indirubin and methanol, applied in the directions of organic chemistry, drug combination, antitumor drugs, etc., can solve the problems of unfavorable large-scale production operations, low indirubin content, etc.

Inactive Publication Date: 2010-02-17
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the extraction and separation methods of indirubin mainly include chloroform extraction, ethanol extraction and ethyl acetate extraction, etc., but the content of indirubin obtained by these extraction processes is very low, and it is unfavorable for large-scale production operations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 10Kg of Folium folium, add 5 times the amount of methanol for ultrasonic extraction once, 0.2 hours each time, the ultrasonic frequency is 50KHZ, combine the extracts, recover methanol under reduced pressure and concentrate, the liquid passes through the AB-8 macroporous resin column, first Remove impurities by elution with water, then elute with ethyl acetate, concentrate the eluent, separate by alumina column chromatography, elute with chloroform-ethyl acetate (2:1), concentrate the eluent, and use methanol-acetone ( 1:1) recrystallized, washed and dried to obtain 1.8 g of red powder, which was detected by HPLC with a purity of 95.3%.

Embodiment 2

[0017] Take 10Kg of Folium folium, add 10 times the amount of methanol and ultrasonically extract 3 times, each time for 1 hour, the ultrasonic frequency is 50KHZ, combine the extracts, recover methanol under reduced pressure and concentrate, the drug solution passes through the H-103 macroporous resin column, first Remove impurities by elution with water, then elute with ethyl acetate, concentrate the eluent, separate by alumina column chromatography, elute with chloroform-ethyl acetate (7:1), concentrate the eluent, and use methanol-acetone ( 1:3) recrystallized, washed and dried to obtain 2.6 g of red powder, which was detected by HPLC with a purity of 93.2%.

Embodiment 3

[0019] Take 10Kg of Folium folium, add 8 times the amount of methanol for ultrasonic extraction twice, each time for 0.5 hours, the ultrasonic frequency is 50KHZ, combine the extracts, recover methanol under reduced pressure and concentrate, the liquid is passed through a D-101 macroporous resin column, first Remove impurities by elution with water, then elute with ethyl acetate, concentrate the eluent, separate by alumina column chromatography, elute with chloroform-ethyl acetate (5:1), concentrate the eluent, and use methanol-acetone ( 1:2) recrystallization, washing, and drying to obtain 2.4 g of red powder, which was detected by HPLC with a purity of 98.1%.

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PUM

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Abstract

The invention relates to a method for preparing indirubin with simple and convenient operation, small pollution and little equipment investment. The method comprises the following technological steps:adding methanol with the quantity of 5-10 times of raw materials into the raw materials, extracting by ultrasonic for 1-3 times, extracting for 0.2-1 hour each time, merging extracting liquid, recovering the methanol by depressurization, concentrating, filtering liquor by a macroporous resin column, eluting with water firstly, removing impurities, then eluting with ethyl acetate, concentrating eluent, adopting chromatographic separation by an alumina column, eluting with chloroform-ethyl acetate, concentrating eluent, recrystallizing with methanol-acetone, washing, drying to obtain the indirubin. By adopting the invention to prepare the indirubin, the product purity is high and industrialization amplification is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing indirubin, in particular to a method for extracting indirubin from plants. Background technique [0002] Indirubin, whose chemical name is 2,2'-biindole-3,3'-dione, is a drug discovered in my country with a chemical structure different from known antineoplastic drugs, mainly found in Daqing Leaves, Banlangen, Qingdai and other Chinese herbal medicines. Its molecular formula is C 15 h 10 N 2 o 2 , the formula weight is 262.26. Indirubin is weakly alkaline, insoluble in water, hardly soluble in cold ethanol, but soluble in ethyl acetate, etc. and is volatile. Indirubin has a good effect on the treatment of chronic myelogenous leukemia. [0003] In the prior art, the extraction and separation methods of indirubin mainly include chloroform extraction, ethanol extraction and ethyl acetate extraction, etc., but the content of indirubin obtained by these extraction processes is very low, and it is not cond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/36A61P35/02
Inventor 王琳范淦彬
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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