CN107253962A - A kind of technique that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor - Google Patents
A kind of technique that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor Download PDFInfo
- Publication number
- CN107253962A CN107253962A CN201710504310.0A CN201710504310A CN107253962A CN 107253962 A CN107253962 A CN 107253962A CN 201710504310 A CN201710504310 A CN 201710504310A CN 107253962 A CN107253962 A CN 107253962A
- Authority
- CN
- China
- Prior art keywords
- dihydroartemisinine
- artesunate
- mother liquor
- crystallization
- hexane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/20—Spiro-condensed systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the technique that dihydroartemisinine is reclaimed in a kind of crystallization from artesunate mother liquor, comprise the following steps：1）With Artesunate synthesis mother liquid it is concentrated and dry remove organic solvent after crystalline powder crystallize for raw material, with organic solvent dissolving mother liquor crystallization obtain material solution；2）By material solution by chromatographic column after, the eluant, eluent for adding ethyl acetate hexane is eluted, and is collected the organic solvent containing dihydroartemisinine and is concentrated, obtains dihydroartemisinine coarse-grain；3）Using dihydroartemisinine coarse-grain as the raw material for recombining Artesunate, the present invention is with preparation technology is simple, organic efficiency is higher, prepare lower-cost advantage in a word.
Description
Technical field
The invention belongs to qinghaosu spin-off preparation technology field, and in particular to be returned in a kind of crystallization from artesunate mother liquor
The technique for receiving dihydroartemisinine.
Background technology
Qinghaosu is that a kind of obtained colourless acicular crystal is extracted from compound inflorescence plant Artemisia annua i.e. Chinese medicine artemisia leaf,
Not pastille sweet wormwood in its stem, qinghaosu is the maximally effective antimalarial specific drug after pyrimethamine, chloroquine, primary quinoline, blue or green in addition
Punt-pole element also shows that tempting prospect in the treatment of other diseases；Such as immunologic function of anti-schistosome, regulation or suppression body fluid,
The conversion ratio of lymphocyte is improved, cholagogic, eliminating the phlegm, antibechic is relievingd asthma；Dihydroartemisinine is the derivative of qinghaosu, former to malaria
Worm erythrocytic stage has powerful and quick killing action, and it synthesizes artesunic using dihydroartemisinine is raw material, in this process
Middle mother liquor produces the dihydroartemisinine containing part in crystallization, this partial mother liquid, and weak is this partial mother liquid not to be handled back
Receive, a large amount of losses of qinghaosu will certainly be caused, and this is related in current art scheme also less.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, and provide and returned in a kind of crystallization from artesunate mother liquor
The technique for receiving dihydroartemisinine.
The object of the present invention is achieved like this：The work of dihydroartemisinine is reclaimed in a kind of crystallization from artesunate mother liquor
Skill, comprises the following steps：
1）With Artesunate synthesis mother liquid it is concentrated and dry remove organic solvent after crystalline powder crystallize for raw material, to have
Machine solvent dissolving mother liquor crystallization obtains material solution；
2）By material solution by chromatographic column after, the eluant, eluent for adding n-hexane-ethyl acetate is eluted, and is collected containing double hydrogen
The organic solvent of qinghaosu is concentrated, and obtains dihydroartemisinine coarse-grain；
3）It regard dihydroartemisinine coarse-grain as the raw material for recombining Artesunate.
Preferably, the step 1）Middle raw material removes for the concentrated drying of mother liquor produced in the production process of Artesunate
Crystalline powder after organic solvent.
Preferably, described rapid 1）In organic solvent be acetone, dichloromethane, chloroform, petroleum ether, methanol, acetic acid
The volume that the solvent is added in ethyl ester or n-hexane, every kilogram of raw material is 32L.
Preferably, described rapid 1）In organic solvent be n-hexane.
Preferably, the step 2）In eluant, eluent be acetone-methanol, petroleum ether-acetone.
Preferably, the eluant, eluent is n-hexane-ethyl acetate intermixture.
Preferably, n-hexane in the n-hexane-ethyl acetate intermixture：The volume ratio of ethyl acetate is 39-147:3.
Preferably, n-hexane in the n-hexane-ethyl acetate intermixture：The volume ratio of ethyl acetate is 97:3.
Preferably, the step 2）In chromatographic column medium be macroreticular resin, aluminum oxide, add in every kilogram of raw material
The weight of medium is 26kg.
Beneficial effects of the present invention：The inventive method is simple and easy to apply, and convenient for production, cost is low, dihydroartemisinine coarse-grain
Yield can reach more than 10%, the mother liquor effectively produced in recycling Artesunate production process, reclaim dihydroartemisinine,
And dihydroartemisinine synthesis Artesunate can be reused, in a word the present invention have that preparation technology is simple, organic efficiency is higher,
Prepare lower-cost advantage.
Embodiment
Embodiment
The technique that dihydroartemisinine is reclaimed in a kind of crystallization from artesunate mother liquor, comprises the following steps：
1）With Artesunate synthesis mother liquid it is concentrated and dry remove organic solvent after crystalline powder crystallize for raw material, to have
Machine solvent dissolving mother liquor crystallization obtains material solution；
2）By material solution by chromatographic column after, the eluant, eluent for adding n-hexane-ethyl acetate is eluted, and is collected containing double hydrogen
The organic solvent of qinghaosu is concentrated, and obtains dihydroartemisinine coarse-grain；
3）It regard dihydroartemisinine coarse-grain as the raw material for recombining Artesunate.
The step 1）Middle raw material is organic molten for the concentrated dry removal of mother liquor produced in the production process of Artesunate
Crystalline powder after agent.
Described rapid 1）In organic solvent be acetone, dichloromethane, chloroform, petroleum ether, methanol, ethyl acetate or just
The volume that the solvent is added in hexane, every kilogram of raw material is 32L.
Described rapid 1）In organic solvent be n-hexane.
The step 2）In eluant, eluent be acetone-methanol, petroleum ether-acetone.
The eluant, eluent is n-hexane-ethyl acetate intermixture.
N-hexane in the n-hexane-ethyl acetate intermixture：The volume ratio of ethyl acetate is 39-147:3.
N-hexane in the n-hexane-ethyl acetate intermixture：The volume ratio of ethyl acetate is 97:3.
The step 2）In chromatographic column medium be macroreticular resin, aluminum oxide, medium is added in every kilogram of raw material
Weight is 26kg.
The present invention is when implementing, and the inventive method is simple and easy to apply, and convenient for production, cost is low, the receipts of dihydroartemisinine coarse-grain
Rate can reach more than 10%, the mother liquor effectively produced in recycling Artesunate production process, reclaim dihydroartemisinine, and
Dihydroartemisinine synthesis Artesunate can be reused, the present invention is with preparation technology is simple, organic efficiency is higher, system in a word
Standby lower-cost advantage.
Claims (9)
1. the technique of dihydroartemisinine is reclaimed in a kind of crystallization from artesunate mother liquor, it is characterised in that：Comprise the following steps：
1）With Artesunate synthesis mother liquid it is concentrated and dry remove organic solvent after crystalline powder crystallize for raw material, to have
Machine solvent dissolving mother liquor crystallization obtains material solution；
2）By material solution by chromatographic column after, the eluant, eluent for adding n-hexane-ethyl acetate is eluted, and is collected containing double hydrogen
The organic solvent of qinghaosu is concentrated, and obtains dihydroartemisinine coarse-grain；
3）It regard dihydroartemisinine coarse-grain as the raw material for recombining Artesunate.
2. reclaiming the method for dihydroartemisinine in a kind of crystallization from artesunate mother liquor as claimed in claim 1, its feature exists
In：The step 1）Middle raw material is removed after organic solvent for the concentrated drying of mother liquor produced in the production process of Artesunate
Crystalline powder.
3. the method for dihydroartemisinine, its feature are reclaimed in a kind of crystallization from artesunate mother liquor as claimed in claim 1 or 2
It is：Described rapid 1）In organic solvent for acetone, dichloromethane, chloroform, petroleum ether, methanol, ethyl acetate or just oneself
The volume that the solvent is added in alkane, every kilogram of raw material is 32L.
4. reclaiming the method for dihydroartemisinine in a kind of crystallization from artesunate mother liquor as claimed in claim 3, its feature exists
In：Described rapid 1）In organic solvent be n-hexane.
5. the method for dihydroartemisinine, its feature are reclaimed in a kind of crystallization from artesunate mother liquor as claimed in claim 1 or 2
It is：The step 2）In eluant, eluent be acetone-methanol, petroleum ether-acetone.
6. the method for dihydroartemisinine, its feature are reclaimed in a kind of crystallization from artesunate mother liquor as claimed in claim 1 or 2
It is：The eluant, eluent is n-hexane-ethyl acetate intermixture.
7. reclaiming the method for dihydroartemisinine in a kind of crystallization from artesunate mother liquor as claimed in claim 6, its feature exists
In：N-hexane in the n-hexane-ethyl acetate intermixture：The volume ratio of ethyl acetate is 39-147:3.
8. reclaiming the method for dihydroartemisinine in a kind of crystallization from artesunate mother liquor as claimed in claim 7, its feature exists
In：N-hexane in the n-hexane-ethyl acetate intermixture：The volume ratio of ethyl acetate is 97:3.
9. the method for dihydroartemisinine, its feature are reclaimed in a kind of crystallization from artesunate mother liquor as claimed in claim 1 or 2
It is：The step 2）In chromatographic column medium be macroreticular resin, aluminum oxide, the weight of medium is added in every kilogram of raw material
For 26kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710504310.0A CN107253962A (en) | 2017-06-28 | 2017-06-28 | A kind of technique that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710504310.0A CN107253962A (en) | 2017-06-28 | 2017-06-28 | A kind of technique that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107253962A true CN107253962A (en) | 2017-10-17 |
Family
ID=60024338
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710504310.0A Pending CN107253962A (en) | 2017-06-28 | 2017-06-28 | A kind of technique that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107253962A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543198A (en) * | 2016-08-31 | 2017-03-29 | 重庆华方武陵山制药有限公司 | A kind of method that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
-
2017
- 2017-06-28 CN CN201710504310.0A patent/CN107253962A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543198A (en) * | 2016-08-31 | 2017-03-29 | 重庆华方武陵山制药有限公司 | A kind of method that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2020228786A1 (en) | Industrialized method for rapidly and efficiently extracting xanthophyll and quercetagetin | |
| CN104292238A (en) | Method for extracting sesamin from sesame cake meals | |
| CN107312015A (en) | A kind of technique of efficiently extracting and producing artemisinin by ionic liquid | |
| CN103896955B (en) | A kind of method extracting sesamin from sesame oil | |
| CN102887926A (en) | Method for extracting aucubin from eucommia ulmoides seed meal | |
| CN107253962A (en) | A kind of technique that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor | |
| US8765196B2 (en) | Method for separating and purifying Ginkgolide C from root bark of ginkgo | |
| CN110078610B (en) | Preparation method of 6-gingerol | |
| CN100595193C (en) | Industrial method for producing natural capsicine | |
| WO2016082059A1 (en) | Method for extracting artemisinin by aqueous solution ultrasound | |
| CN104987952B (en) | Method for extracting volatile oil and salidroside from rhodiola rosea whole plant | |
| CN111171104A (en) | Method for preparing ursolic acid from rosemary oil paste by-product | |
| CN101412724B (en) | Method for extracting bilobalide compound from ginkgo leaf | |
| CN106905339B (en) | Method for purifying phillygenin from forsythia suspense leaves | |
| CN103012071A (en) | Method for extracting and purifying resveratrol from peanut meal | |
| CN109280065B (en) | Method for extracting and separating mangiferin | |
| EP3511326A1 (en) | Method for preparing voriconazole l-camphorsulphonate and voriconazole | |
| CN106431895A (en) | Method for extracting lactic acid from fermentation liquor through combination of molecular distillation and extraction | |
| CN112358526A (en) | Method for preparing citrus seed limonin from citrus seeds | |
| CN107383047B (en) | Method for extracting artemisinin | |
| KR102556971B1 (en) | A new synthesis method of (+)-Decursinol | |
| CN106588848B (en) | The method of luteolin is extracted in a kind of peanut shell | |
| CN102627540A (en) | Alnustone purification method | |
| CN117105949B (en) | Method for preparing high-purity glabridin by using melt crystallization | |
| CN108752397A (en) | A kind of extracting method of amarogentin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171017 |
|
| RJ01 | Rejection of invention patent application after publication |