CN103435583A - Preparation method for 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone - Google Patents
Preparation method for 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone Download PDFInfo
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- CN103435583A CN103435583A CN2013103601299A CN201310360129A CN103435583A CN 103435583 A CN103435583 A CN 103435583A CN 2013103601299 A CN2013103601299 A CN 2013103601299A CN 201310360129 A CN201310360129 A CN 201310360129A CN 103435583 A CN103435583 A CN 103435583A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a preparation method with easy and convenient operation and little pollution for 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone. The preparation method comprises the following steps: 1) taking and smashing dry incarvillea arguta leaves; sieving the smashed incarvillea arguta leaves by a sieve with 20-80 meshes; placing the sieved incarvillea arguta leaves into a supercritical CO2 extraction pot for extraction, wherein the flow rate of CO2 is 1-3 ml/min/g raw material, the extraction temperature is 30-60 DEG C, the pressure is 15-30 MPa, and the extraction time is 60-200 min: analyzing to obtain an extract; 2) dissolving the extract in a 60%-90% methanol solution; adding petrolic ether with the same volumn as that of the methanol solution for extracting; removing a petrolic ether layer; using a chloroform solution for extracting again; collecting chloroform layer concentration crystals; adding absolute ethyl alcohol into the crystal substances for recrystallization, drying crystal substances at low temperature to obtain the 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone. Through the adoption of the method to produce the 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone, the obtained product is high in purity, and the industrialisation is easy to realize.
Description
Technical field
The invention belongs to biological technical field, especially relate to a kind of preparation method of Westerner's humulone.
Background technology
Westerner's grass is again suona horn flower, the Bignoniaceae plant, bitter, cool, have dispel rheumatism, the effect of anti-inflammatory analgetic, promoting blood circulation to remove blood stasis.The modern study discovery, contain alkaloid, flavonoid and terpene substances in Westerner's grass, wherein Westerner's humulone is medicinal composition in Westerner's grass, has antibiotic, antivirus action.
Westerner's humulone chemical name 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone, molecular formula C8H10O5, molecular weight 186.17,94 ℃ of mp (distillation), be soluble in trichloromethane, methyl alcohol; Be dissolved in benzene, ether, acetone, ethyl acetate and ethanol; Water insoluble.
By literature search, the preparation method of existing Westerner's humulone adopts normal pressure to extract and silica gel column chromatography more, the method complicated operation, and solvent load is large, and product yield is low, and technique is difficult for realizing industrialization.
Summary of the invention
The objective of the invention is to solve prior art deficiency and defect, a kind of preparation method of Westerner's humulone simple to operate is provided.
The objective of the invention is to realize by the following technical solutions: a kind of preparation method of Westerner's humulone is characterized in that comprising following steps:
1) get dry Westerner's blade of grass and pulverize the 20-80 order, be placed in the SCF-CO 2 tank and extract, the CO2 flow is the 1-3ml/min/g raw material, extraction temperature 30-60 ℃, and pressure 15-30Mpa, extraction time 60-200min, resolve to obtain extract;
2) above-mentioned extract 60%-90% dissolve with methanol solution, add the equal-volume petroleum ether extraction, removes petroleum ether layer, then, with chloroformic solution extraction, collect the chloroform layer condensing crystal, and crystallisate adds the dehydrated alcohol recrystallization, crystallisate cryodrying and get final product.
SCF-CO 2 condition in step 1) is: the CO2 flow is the 2ml/min/g raw material, 40 ℃ of extraction temperature, pressure 18Mpa, extraction time 120min.
Adopt present method to prepare Westerner's humulone, extraction efficiency is high, pollutes littlely, and product yield is high, simple to operate, is easy to suitability for industrialized production.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
embodiment:
Embodiment 1:
Get dry Westerner's blade of grass and pulverize 40 orders, get 5kg, being placed in the SCF-CO 2 tank extracts, passing into the CO2 flow is the 2ml/min/g raw material, 40 ℃ of extraction temperature, pressure 18Mpa, extraction time 120min, resolve 300ml80% methanol solution heating for dissolving for extract, add the equal-volume petroleum ether extraction 3 times, remove petroleum ether layer, solution is again with 200ml chloroformic solution extraction 3 times, collect chloroform layer to 30ml, the refrigeration crystallization, crystallisate leaches and adds 50ml dehydrated alcohol backflow dissolving-recrystallization, the crystallisate cryodrying, obtain Westerner's humulone 7.3g, through HPLC, detect, content 98.5%.
Embodiment 2:
Get dry Westerner's blade of grass and pulverize 60 orders, get 5kg, being placed in the SCF-CO 2 tank extracts, passing into the CO2 flow is the 3ml/min/g raw material, 30 ℃ of extraction temperature, pressure 15Mpa, extraction time 100min, resolve 300ml90% methanol solution heating for dissolving for extract, add the equal-volume petroleum ether extraction 2 times, remove petroleum ether layer, solution is again with 100ml chloroformic solution extraction 4 times, collect chloroform layer to 25ml, the refrigeration crystallization, crystallisate leaches and adds 70ml dehydrated alcohol backflow dissolving-recrystallization, the crystallisate cryodrying, obtain Westerner's humulone 7.9g, through HPLC, detect, content 96.9%.
Embodiment 3:
Get dry Westerner's blade of grass and pulverize 80 orders, get 5kg, being placed in the SCF-CO 2 tank extracts, passing into the CO2 flow is the 1ml/min/g raw material, 60 ℃ of extraction temperature, pressure 30Mpa, extraction time 120min, resolve 200ml60% methanol solution heating for dissolving for extract, add the equal-volume petroleum ether extraction 4 times, remove petroleum ether layer, solution is again with 300ml chloroformic solution extraction 3 times, collect chloroform layer to 40ml, the refrigeration crystallization, crystallisate leaches and adds 100ml dehydrated alcohol backflow dissolving-recrystallization, the crystallisate cryodrying, obtain Westerner's humulone 7.7g, through HPLC, detect, content 97.4%.
Claims (2)
1. the preparation method of Westerner's humulone is characterized in that comprising following steps:
1) get dry Westerner's blade of grass and pulverize the 20-80 order, be placed in the SCF-CO 2 tank and extract, the CO2 flow is the 1-3ml/min/g raw material, extraction temperature 30-60 ℃, and pressure 15-30Mpa, extraction time 60-200min, resolve to obtain extract;
2) above-mentioned extract 60%-90% dissolve with methanol solution, add the equal-volume petroleum ether extraction, removes petroleum ether layer, then, with chloroformic solution extraction, collect the chloroform layer condensing crystal, and crystallisate adds the dehydrated alcohol recrystallization, crystallisate cryodrying and get final product.
2. the preparation method of Westerner's humulone as claimed in claim 1, it is characterized in that the SCF-CO 2 condition in described step 1) is: the CO2 flow is the 2ml/min/g raw material, 40 ℃ of extraction temperature, pressure 18Mpa, extraction time 120min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103601299A CN103435583A (en) | 2013-08-19 | 2013-08-19 | Preparation method for 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013103601299A CN103435583A (en) | 2013-08-19 | 2013-08-19 | Preparation method for 2-Ethoxymethylene-3,5-dihydroxy-y-pyrone |
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| CN103435583A true CN103435583A (en) | 2013-12-11 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788041A (en) * | 2014-03-25 | 2014-05-14 | 南通奥凯生物技术开发有限公司 | Method for purifying sodium dehydroacetate |
| CN104830954A (en) * | 2015-06-04 | 2015-08-12 | 辛本勤 | N.braziliensis selective medium for pleural effusion sample |
-
2013
- 2013-08-19 CN CN2013103601299A patent/CN103435583A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788041A (en) * | 2014-03-25 | 2014-05-14 | 南通奥凯生物技术开发有限公司 | Method for purifying sodium dehydroacetate |
| CN104830954A (en) * | 2015-06-04 | 2015-08-12 | 辛本勤 | N.braziliensis selective medium for pleural effusion sample |
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| PB01 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131211 |