Preparation method of ailanthinone

A technology of Ailanthus ketone and Ailanthus ailanthus, which is applied in the field of preparation of Ailanthus ketone extracted from plants, achieves the effects of less pollution, less energy consumption, and is conducive to large-scale production operations

Inactive Publication Date: 2010-09-15
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no preparation process report suitable for industrialized large-scale production of Ailanthus ketone

Method used

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  • Preparation method of ailanthinone

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Experimental program
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Effect test

Embodiment 1

[0018] Take 10Kg of fresh bark of Ailanthus sinensis, add 5 times its mass and volume of ammonia solution with pH=9, soak for 24 hours, filter, adjust the pH of the filtrate to neutral with hydrochloric acid, concentrate, and pass the concentrated solution through AB-8 macroporous adsorption resin Column adsorption, water elution to remove impurities, 60% ethanol elution, collect 3 times the column volume eluate, recover ethanol under reduced pressure to the end, refrigerate for 12 hours to crystallize, filter, take the filter residue, add acetone for recrystallization, wash, After drying, 1.23 g of Ailanthione was obtained, and the purity was 98.2% as detected by HPLC.

Embodiment 2

[0020] Take 10Kg of fresh bark of Ailanthus sinensis, add 10 times its mass and volume of pH=13 KOH aqueous solution, soak for 72 hours, filter, adjust the pH of the filtrate to neutral with hydrochloric acid, concentrate, and pass the concentrated solution through AB-8 macroporous adsorption resin column Adsorption, water elution to remove impurities, 85% ethanol elution, collect 8 times the column volume eluate, recover ethanol under reduced pressure to the end, refrigerate for 36 hours to crystallize, filter, take the filter residue, add acetone for recrystallization, wash and dry That is, 1.62 g of Ailanthonone was obtained, and the purity was 97.4% as detected by HPLC.

Embodiment 3

[0022] Take 10Kg of fresh bark of Ailanthus sinensis, add 8 times its mass and volume of NaOH aqueous solution with pH=10, soak for 36 hours, filter, adjust the pH of the filtrate to neutral with hydrochloric acid, concentrate, and pass the concentrated solution through AB-8 macroporous adsorption resin column Adsorption, water elution to remove impurities, 80% ethanol elution, collect 5 times the column volume eluate, recover ethanol under reduced pressure to the end, refrigerate for 24 hours to crystallize, filter, take the filter residue, add acetone for recrystallization, wash and dry That is, 1.54 g of Ailanthus ketone was obtained, and the purity was 98.8% as detected by HPLC.

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Abstract

The invention relates to a preparation method of ailanthinone, with convenient operation, small pollution and less energy consumption. The preparation method comprises the processing steps of: taking the fresh bark or the fresh velamen of ailanthus, and adding water containing soda the volume of which is 5-10 times of the weight of the fresh bark or the fresh velamen of ailanthus and the pH of which is 9-13 to soak the fresh bark or the fresh velamen of ailanthus for 24-72 hours; filtering; regulating filter liquor until pH to be neutral; concentrating; absorbing concentrated liquor with macroporous adsorbent resins; washing with water to remove impurities; washing with 60-85 percent of ethanol; collecting 3-8 time column volume of eluent; recovering the ethanol under decompression until no ethanol remains; refrigerating for 12-36 hours for devitrification; filtering; taking filter residues and adding acetone for recrystallization; washing and then drying to obtain the ailanthinone. The ailanthinone prepared by adopting the invention has high purity, and industrial amplification is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of ailanthonone, in particular to a preparation method of extracting ailanthonone from plants. Background technique [0002] Ailanthone, also known as Ailanthus ketone, molecular formula: C20H24O7, molecular weight: 376.405, CAS accession number: 981-15-7, mainly exists in the seeds and root bark of Ailanthus altissima (Mill.) Swingle , In the bark. Its molecular formula is as follows: [0003] [0004] Modern research shows that Ailanthus ketone has anti-amoebic dysentery, anti-malarial, anti-ulcer, inhibition of gastric acid secretion, etc., and it is also used as a raw material for the synthesis of other active derivatives. [0005] In the prior art, there is no report on the preparation process suitable for the large-scale industrial production of Ailanthus ketone. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a method for preparing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/20
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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