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Preparation method of demethylwedelolactone

A technology of norwerethrin and methanol solution is applied in the field of natural medicinal chemistry and can solve problems such as non-specificity and the like

Inactive Publication Date: 2013-08-28
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as "Studies on the Chemical Components of Eclipta" This document uses silica gel column to separate various components in Eclipta, and the method is not specific

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Crush Eclipta leaves, weigh 2kg, extract 3 times with 10L50% methanol solution ultrasonically for 30 minutes each time, concentrate the extract under reduced pressure to 1000ml, add an equal volume of ethyl acetate to extract 3 times, combine the extracts to recover ethyl acetate get the extract. Add an appropriate amount of hot water to the extract, stir it, add it to the HZ816 macroporous resin column for adsorption, and elute with 10 times the column volume of 50% methanol solution. Take petroleum ether, ethyl acetate, methanol, and water, mix them according to 2:4:5:4, and after fully layering, take the upper phase and fill the high-speed countercurrent chromatography tube as the stationary phase, turn on the main engine at a speed of 900rpm, and pump in at the same time The lower phase is used for flow phasing. After the dynamic balance is established, the flow rate is adjusted to 2ml / min. The crude extract is dissolved with the mobile phase, and the sample is inje...

Embodiment 2

[0017] Crush the leaves of Eclipta chinensis, weigh 2kg, use 16L 60% methanol solution for ultrasonic extraction for 40 minutes each time, extract twice, concentrate the extract under reduced pressure to 900ml, add an equal volume of ethyl acetate to extract three times, combine the extracts to recover ethyl acetate get the extract. The extract was added to an ADS-21 macroporous resin column for adsorption with appropriate amount of hot water, and eluted with 50% methanol solution 15 times the column volume. Take petroleum ether, ethyl acetate, methanol, and water, mix them according to 3:7:7:5, and after fully layering, take the upper phase and fill the high-speed countercurrent chromatography tube as the stationary phase, turn on the main engine at a speed of 850rpm, and pump in at the same time The lower phase is used for flow phasing. After the dynamic balance is established, the flow rate is adjusted to 3ml / min, and the crude extract is dissolved with the mobile phase. Th...

Embodiment 3

[0019] Crush the leaves of Eclipta chinensis, weigh 2kg, extract 3 times with 14L 70% methanol solution ultrasonically for 30 minutes each time, concentrate the extract under reduced pressure to 800ml, add an equal volume of ethyl acetate to extract 3 times, combine the extracts to recover ethyl acetate get the extract. Add an appropriate amount of hot water to the extract, stir it, add it to a HPD100 macroporous resin column for adsorption, and elute with 13 times the column volume of 50% methanol solution. Take petroleum ether, ethyl acetate, methanol, and water, mix them according to 5:4:5:9, and after fully layering, take the upper phase and fill the high-speed countercurrent chromatography tube as the stationary phase, turn on the main engine at a speed of 700rpm, and pump in at the same time The lower phase is used for flow phasing. After the dynamic balance is established, the flow rate is adjusted to 1ml / min. The crude extract is dissolved with the mobile phase, and th...

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PUM

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Abstract

The invention discloses a preparation method of demethylwedelolactone, which is simple and convenient to operate and small in pollution. The method comprises the following steps of: crushing an eclipta raw material; adding 5-10 times of 40-70% methanol liquor for ultrasonic extraction for 2-3 times; concentrating the extracting liquor and extracting by ethyl acetate liquor; collecting the extract recovering reagent, adding macroporous resin to adsorb, and eluting by 5-10 times of 50% methanol liquor in volume; concentrating the eluent to obtain a crude extract; and then, separating by high speed counter current chromatography, online monitoring by an ultraviolet detector and collecting the fraction and decompressing and drying to obtain demethylwedelolactone. According to the method for preparing demethylwedelolactone, the purity of the product obtained is high, and the method is beneficial for industrial amplification.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a preparation method of norwedelolide. Background technique [0002] Norwedelide, CAS No. 6468-55-9, molecular formula C 15 h 8 o 7 , the molecular weight is 300.2, and the molecular structure formula is as follows: [0003] . [0004] Norwedelolide is a kind of coumarin compound isolated from Eclipta japonica, which has anti-inflammatory and anti-stem cell toxicity effects. [0005] Eclipta chinensis is the whole herb of the snakehead sausage, and its leaves contain wedelide and norwedelide. Desmethylwedelolide-7-glucoside. The leaves contain wedelolactone, demethylwedelolactone and demethylwedelolactone glucoside. [0006] Through literature search, there is no disclosure of the preparation method of norwedelide. Such as "Research on the Chemical Components of Eclipta" this document uses a silica gel column to separate various components in Eclipta, and the ...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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