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A kind of preparation method of 2'-hydroxy pterophyll

A technology of fern and hydroxyl, which is applied in the field of preparation of 2'-hydroxy fernol, which achieves the effects of less pollution, favorable large-scale production operations, and low energy consumption

Inactive Publication Date: 2011-12-07
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity 2'-hydroxypiperinol

Method used

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  • A kind of preparation method of 2'-hydroxy pterophyll

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 10Kg of rhizome of oriental viburnum, crush it, add 80L of ethanol with a concentration of 50%, put it into a microwave extraction device for microwave extraction, extraction power 300W, extract once, 3 minutes, combine the extracts, filter, and recover ethanol under reduced pressure And concentrated, added to HPD-700 macroporous adsorption resin column, eluted with 30% ethanol, collected 3 times the column volume of eluent, recovered ethanol under reduced pressure and concentrated, added to nylon 6 (polycaprolactam) On the polyamide chromatography column, the dichloromethane-methanol mixed solvent with a ratio of 5:3 was used as the eluent to elute, and the same type of polyamide film was developed with the above eluent as a supporting detection, and the corresponding polyamide was collected. For fractions with Rf=4-5 on the film, the solvent was recovered under reduced pressure, methanol was added to crystallize, the crystals were separated, washed and dried to ob...

Embodiment 2

[0027] Take 10Kg of oriental pod fern rhizome, crush it, add 120L of ethanol with a concentration of 70%, put it into a microwave extraction device for microwave extraction, extraction power 600W, extract 3 times, each time for 10 minutes, combine the extracts, filter, and reduce pressure Recover ethanol and concentrate, add to H-50 macroporous adsorption resin column, elute with 50% ethanol, collect eluate with 8 times the column volume, recover ethanol under reduced pressure and concentrate, add to nylon 66 (polyhexane Hexamethylene diamide) polyamide chromatography column, elute with dichloromethane-methanol mixed solvent with a ratio of 5:3 as eluent, use the same type of polyamide film to develop with the above eluent as a supporting detection, Collect the fractions corresponding to Rf=4-5 on the polyamide film, recover the solvent under reduced pressure, add methanol to crystallize, separate the crystals, wash and dry to obtain 20.3g of 2'-hydroxypterinol, which was detec...

Embodiment 3

[0029] Take 10Kg of oriental pod fern rhizome, crush it, add 100L of ethanol with a concentration of 60%, put it into a microwave extraction device for microwave extraction, extraction power is 500W, extract twice, each time for 8 minutes, combine the extracts, filter, and decompress Recover ethanol and concentrate, add to CD-180 macroporous adsorption resin column, elute with 40% ethanol, collect eluate with 5 times the column volume, recover ethanol under reduced pressure and concentrate, add to nylon 66 (polyhexane Hexamethylene diamide) polyamide chromatography column, elute with dichloromethane-methanol mixed solvent with a ratio of 5:3 as eluent, use the same type of polyamide film to develop with the above eluent as a supporting detection, Collect the fractions corresponding to Rf=4-5 on the polyamide film, recover the solvent under reduced pressure, add methanol to crystallize, separate the crystals, wash and dry to obtain 18.9g of 2'-hydroxypterinol, which was detected...

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Abstract

The present invention relates to a preparation method of 2'-hydroxyporphyrin with simple and convenient operation, little pollution and low energy consumption. The process steps are: take the rhizome of oriental viburnum, crush it, add ethanol, put it into a microwave extraction device for microwave extraction, combine the extracts, filter, recover ethanol under reduced pressure and concentrate, add it to a macroporous adsorption resin column, 30-50 % ethanol for elution, ethanol is recovered under reduced pressure and concentrated, added to a polyamide chromatography column, eluted with a mixed solvent of dichloromethane-methanol at a ratio of 5:3, recovered under reduced pressure, and crystallized by adding methanol , separate the crystals, wash and dry. The preparation of 2'-hydroxypteria phenol by the present invention has high product purity and is easy to realize industrial scale-up.

Description

technical field [0001] The present invention relates to a preparation method of 2'-hydroxypiabolol, in particular to a preparation method of extracting 2'-hydroxypembrolol from plants. Background technique [0002] 2'-Hydroxymatteucinol (2'-Hydroxymatteucinol), molecular formula: C 18 h 18 o 6 , Molecular weight: 330.337, CAS accession number: 154320-34-0, mainly exists in a variety of plants of Tridentaceae. Pteridophyllum orientalis Matteuccia orientalis (Hook.) Trev. is rich in content, and its molecular formula is as follows. [0003] [0004] Modern studies have shown that 2'-hydroxypiperinol has a strong hypoglycemic effect, and it is also used as a raw material for the synthesis of other active derivatives. [0005] Oriental viburnum Matteuccia orientalis (Hook.) The rhizome of Trev. is used as a traditional Chinese medicine oriental viburnum, which can dispel wind and stop bleeding. [0006] In the prior art, there is no report on the preparation process ...

Claims

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Application Information

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IPC IPC(8): C07D311/32C07D311/40
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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