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A kind of preparation method of ascarin derivative

A technology for astragalosides and derivatives, which is applied in the preparation of sugar derivatives, sugar derivatives, sugar derivatives, etc., achieves the effects of low cost, efficient preparation process, and flexible and standardized operation process

Inactive Publication Date: 2020-07-28
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some scientific research teams at home and abroad have conducted some research on the chemical components of the heartwood, leaves, bark and other parts of the Lianxiang tree (Lee & Bae, Journal of Korean Wood Science and Technology, 2015, 43 (5): 558-565 ; Wang Jingrong, et al., Acta Bot, 1991, 41(2): 209~212; Lee, et al., Journal of Korean WoodScience and Technology, 2016, 44(4): 551~558), however, so far, the The research and reports on the secondary metabolites in the roots of the cypress tree are still extremely rare

Method used

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Examples

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Effect test

Embodiment 1

[0021] Example 1: Preparation of 8-methoxy-4'-O-trans-caffeoylshivetinoside from the root of Lianxiang tree

[0022] Step 1: Take the raw material of the root plant of the syringa japonica that has been dried in the shade, grind it, and add petroleum ether-acetone-water solution with a volume ratio of 3:5:2 according to the mass ratio of material to liquid of 1:3, and heat and extract 3 times, each time 12 hour, the extract was filtered, and the filtrate was concentrated under reduced pressure to 6% of the volume of the extract to obtain the crude extract of the roots of C.

[0023] Step 2: Add water with 4 times the mass of the crude extract, stir, add dichloromethane with 4 times the mass of the crude extract to extract 3 times, separate the dichloromethane layer, add 4 times the mass of the crude extract to the remaining water layer Extract with ethyl acetate for 3 times, separate the ethyl acetate layer, add n-butanol which is 4 times the mass of the crude extract to the r...

Embodiment 2

[0025] Example 2: Preparation of 8-methoxy-4'-O-trans-caffeoylshivetinoside from the root of Lianxiang tree

[0026] Step 1: Take the raw material of the root plant of the syringa japonica that has been dried in the shade, crush it, add petroleum ether-acetone-water solution with a volume ratio of 3:5:2 according to the mass ratio of material to liquid of 1:4, and extract 4 times at normal temperature, each time 72 hour, the extract was filtered, and the filtrate was concentrated under reduced pressure to 8% of the volume of the extract to obtain the crude extract of the roots of C.

[0027] Step 2: Add water with 3 times the mass of the crude extract, stir, add dichloromethane with 3 times the mass of the crude extract to extract 3 times, separate the dichloromethane layer, and add 3 times the mass of the crude extract to the remaining water layer Extract with ethyl acetate for 3 times, separate the ethyl acetate layer, add n-butanol which is 3 times the mass of the crude ext...

Embodiment 3

[0033] Example 3: Preparation of 8-methoxy-4'-O-trans-caffeoylshivetinoside from the root of Lianxiang tree

[0034] Step 1: Take the raw material of the root plant of the syringa japonica tree that has been dried in the shade, and after crushing, add petroleum ether-acetone-water solution with a volume ratio of 3:5:2 according to the mass ratio of material to liquid at 1:2, and extract 3 times with the aid of ultrasonic waves, each time After 0.5 hours, the extract was filtered, and the filtrate was concentrated under reduced pressure to 10% of the volume of the extract to obtain the crude extract of the root of Cinnamomum sinensis;

[0035] Step 2: Add water with 2 times the mass of the crude extract, stir, add dichloromethane with 2 times the mass of the crude extract to extract twice, separate the dichloromethane layer, and add 2 times the mass of the crude extract to the remaining water layer Extracted twice with ethyl acetate, separated the ethyl acetate layer, added n-but...

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Abstract

The invention belongs to the field of high-efficiency preparation of high added value chemical components of wood, and specifically relates to a kaempferol-3-glucoside derivative, namely 8-methoxy-4'-O-trans-caffeoyl kaempferol-3-glucoside which is never reported in published documents, and a preparation technology for preparing the 8-methoxy-4'-O-trans-caffeoyl kaempferol-3-glucoside by combining mixed solution extraction, continuous elution of different polar solvents and high-speed countercurrent chromatography separation. The preparation technology disclosed by the invention has the characteristics of cleanness, high efficiency, high prepared product purity, simpleness in operation, convenience in popularization and application and the like.

Description

technical field [0001] The invention belongs to the field of preparation of high value-added chemical components of forest trees, and in particular relates to a kind of ascarin derivative that has never been reported in the literature, that is, 8-methoxy-4'-O-trans-caffeoyl ascarin (The English name corresponding to the compound is 8-methoxy-4'-O-trans-caffeoylastragalin) and a high-efficiency preparation method thereof. Background technique [0002] Cercidiphyllum japonicum is a plant of the genus Cercidiphyllum in the family Cercidiphyllaceae. It is commonly known as Cercidiphyllum japonicum, and is a precious and rare tree species left over from the Tertiary period. Lianxiang tree is a deciduous tree, which is mainly distributed in China, North Japan, North Korea and South Korea in East Asia. Lianxiangshu flowers are unisexual, without perianth, open first or at the same time as leaves, purplish red, with 1 bract. Male inflorescences are often clustered with 4, nearly s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/07C07H1/08
CPCC07H1/08C07H17/07
Inventor 司传领杨翔皓王蕊
Owner TIANJIN UNIV OF SCI & TECH
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