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Method for preparing vernodalol

A technology of vernonol and anthelmintic vernonia is applied in the field of preparation of vernonia alcohol and achieves the effects of being beneficial to large-scale production operations, low in energy consumption and low in pollution

Inactive Publication Date: 2011-02-02
南京璇荣贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity vernitol

Method used

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  • Method for preparing vernodalol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 10Kg of insect-repelling Vernonia seeds, add water 3 times its mass and volume, and put it into a microwave extraction device for microwave extraction. The extraction power is 300W, and the extraction is performed once for 3 minutes. The extract is collected, the ethanol is recovered under reduced pressure and concentrated, and added to On AB8 macroporous adsorption resin, elute with 40% ethanol, collect 3 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add chloroform to crystallize, separate crystallization, wash and dry to obtain colorless needle crystals - Turtledove 23.67g of chrysanthemum, detected by HPLC, has a purity of 93.6%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 2

[0026] Take 10Kg of insect-repelling Vernonia seeds, add water 8 times its mass and volume, and put it into a microwave extraction device for microwave extraction, extraction power 600W, extraction 3 times, each time 10 minutes, combine the extracts, recover ethanol under reduced pressure and concentrate, Add to D102 type macroporous adsorption resin, elute with 80% ethanol, collect 8 times column volume eluate, recover ethanol under reduced pressure and concentrate, add chloroform to crystallize, separate crystal, wash and dry to obtain colorless needle crystal - 27.13g of vernenol, detected by HPLC, the purity is 90.4%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

Embodiment 3

[0028] Take 10Kg of insect-repelling Vernonia seeds, add water 5 times its mass and volume, and put it into a microwave extraction device for microwave extraction, extraction power 400W, extraction 2 times, 8 minutes each time, combine the extracts, recover ethanol under reduced pressure and concentrate, Add it to D101 macroporous adsorption resin, elute with 60% ethanol, collect 5 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add chloroform to crystallize, separate the crystals, wash and dry to obtain colorless needle crystals - Verninol 25.77g, detected by HPLC, the purity is 96.4%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.

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Abstract

The invention discloses a method for preparing vernodalol, which has advantages of simple and convenient operation, little pollution and low energy consumption. The method comprises the following steps: performing microwave extraction on vernonia anthelmintica seeds in a microwave extraction device; merging the extraction liquid, reducing pressure to recycle ethanol and concentrating; adding to macroporous adsorption resin, eluting by 40 to 80% ethanol and collecting eluant of 3 to 8 times volume; reducing pressure to recycle the ethanol and concentrating; adding chloroform and crystallizing; separating and crystallizing; and washing and drying to obtain the vernodalol. The method for preparing the vernodalol has the advantages of high product purity and easy realization of industrial amplification.

Description

technical field [0001] The invention relates to a preparation method of verninol, in particular to a preparation method of extracting verninol from plants. Background technique [0002] Vernodalol, molecular formula: C 20 h 24 o 8 , molecular weight: 392.405, CAS accession number: 65388-17-2, mainly found in Vernonia anthelmintica Willd. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that vernitol has a strong inhibitory effect on leukemia cells, 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 a preparation process suitable for the industrialized large-scale production of high-purity vernitol. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a method for preparing vernitol which is beneficial to large-scale production operations and has high product purity. [0007] In order to solve the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/02
Inventor 张发成毛志英
Owner 南京璇荣贸易有限公司
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