CN1775755A - Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process - Google Patents
Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process Download PDFInfo
- Publication number
- CN1775755A CN1775755A CN 200510122954 CN200510122954A CN1775755A CN 1775755 A CN1775755 A CN 1775755A CN 200510122954 CN200510122954 CN 200510122954 CN 200510122954 A CN200510122954 A CN 200510122954A CN 1775755 A CN1775755 A CN 1775755A
- Authority
- CN
- China
- Prior art keywords
- pleuromutilin
- tiamulin
- raw material
- building
- preparation
- 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.)
- Granted
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- ZRZNJUXESFHSIO-UHFFFAOYSA-N Pleuromutilin Natural products CC1C(O)C(C)(C=C)CC(OC(=O)CO)C2(C)C(C)CCC31C2C(=O)CC3 ZRZNJUXESFHSIO-UHFFFAOYSA-N 0.000 title claims abstract description 22
- ZRZNJUXESFHSIO-VYTKZBNOSA-N pleuromutilin Chemical compound C([C@H]([C@]1(C)[C@@H](C[C@@](C)(C=C)[C@@H](O)[C@@H]2C)OC(=O)CO)C)C[C@]32[C@H]1C(=O)CC3 ZRZNJUXESFHSIO-VYTKZBNOSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000002994 raw material Substances 0.000 title claims abstract description 10
- UURAUHCOJAIIRQ-QGLSALSOSA-N tiamulin Chemical compound CCN(CC)CCSCC(=O)O[C@@H]1C[C@@](C)(C=C)[C@@H](O)[C@H](C)[C@@]23CC[C@@H](C)[C@]1(C)[C@@H]2C(=O)CC3 UURAUHCOJAIIRQ-QGLSALSOSA-N 0.000 title claims description 12
- 229960004885 tiamulin Drugs 0.000 title claims description 12
- 230000002194 synthesizing effect Effects 0.000 title abstract 2
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 3
- 238000007701 flash-distillation Methods 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- WSGCRAOTEDLMFQ-UHFFFAOYSA-N nonan-5-one Chemical compound CCCCC(=O)CCCC WSGCRAOTEDLMFQ-UHFFFAOYSA-N 0.000 claims description 3
- 241001052560 Thallis Species 0.000 abstract 2
- XYYMFUCZDNNGFS-UHFFFAOYSA-N 2-methylheptan-3-one Chemical compound CCCCC(=O)C(C)C XYYMFUCZDNNGFS-UHFFFAOYSA-N 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing Pleuromutilin raw material used in the course of synthesizing Thiamutin, comprising the steps: drying the wet thalli containing the Pleuromutilin to obtain dry thalli, then making extraction at normal temperature by using methyl ethyl butyl ketone as menstruum, filtering the extracted liquid, discarding filter residues, concentrating the filtrate and obtaining Pleuromutilin concentrate. The invention has high Thiamutin yield, is easy to operate and only uses a kind of menstruum.
Description
Technical field:
The present invention relates to the preparation method of the pleuromutilin of the synthetic usefulness of a kind of Tiamulin.
Background technology:
At present, obtaining of the pleuromutilin raw material of using in the Tiamulin building-up process is that pleuromutilin in the fermented liquid is extracted, and through the centrifugal pleuromutilin that obtains, adds solvent then again, complex process, and also yield is low.
Summary of the invention:
The object of the present invention is to provide a kind of technology simple, yield height, the preparation method of the pleuromutilin raw material of using in the easy-operating Tiamulin building-up process.
Technical solution of the present invention is:
The preparation method of the pleuromutilin raw material of using in a kind of Tiamulin building-up process is characterized in that: comprise the following steps:
To contain the wet thallus drying of pleuromutilin, and obtain dry mycelium, be that solvent extracts at normal temperatures with methyl second butyl ketone again, and the extraction liquid that obtains filters, and abandons filter residue, and concentrating filter liquor obtains the pleuromutilin concentrated solution.
During to the wet thallus drying, adopt flash distillation dryer, inlet temperature is 120～130 ℃, and air outlet temperature is 70～80 ℃.During to the filtrate concentration, temperature is 70～80 ℃, vacuum tightness is-0.05～-0.07MPa.
Technology of the present invention is simple, does not need pleuromutilin is separated, and can directly carry out the synthesis yield height of Tiamulin; Easy to operate; Adopt a kind of solvent, save solvent consumption about 10% than existing technology; The yield height can improve 10～15% than the synthesis yield of existing technology Tiamulin.
The invention will be further described below in conjunction with embodiment.
Embodiment:
The preparation method of the pleuromutilin raw material of using in a kind of Tiamulin building-up process is characterized in that: comprise the following steps:
To contain the wet thallus drying of pleuromutilin, and obtain dry mycelium, be that solvent extracts at normal temperatures with methyl second butyl ketone again, and the extraction liquid that obtains filters, and abandons filter residue, and concentrating filter liquor obtains the pleuromutilin concentrated solution.During to the wet thallus drying, adopt flash distillation dryer, inlet temperature is 120～130 ℃, and air outlet temperature is 70～80 ℃.During to the filtrate concentration, temperature is 70～80 ℃, vacuum tightness is-0.05～-0.07MPa.
Claims (3)
1, the preparation method of the pleuromutilin raw material of using in a kind of Tiamulin building-up process is characterized in that: comprise the following steps:
To contain the wet thallus drying of pleuromutilin, and obtain dry mycelium, be that solvent extracts at normal temperatures with methyl second butyl ketone again, and the extraction liquid that obtains filters, and abandons filter residue, and concentrating filter liquor obtains the pleuromutilin concentrated solution.
2, the preparation method of the pleuromutilin raw material of using in the Tiamulin building-up process according to claim 1 is characterized in that: during to the wet thallus drying, adopt flash distillation dryer, inlet temperature is 120～130 ℃, and air outlet temperature is 70～80 ℃.
3, the preparation method of the pleuromutilin raw material of using in the Tiamulin building-up process according to claim 1 and 2 is characterized in that: during to the filtrate concentration, temperature is 70～80 ℃, vacuum tightness is-0.05～-0.07MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101229540A CN100361976C (en) | 2005-12-06 | 2005-12-06 | Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101229540A CN100361976C (en) | 2005-12-06 | 2005-12-06 | Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1775755A true CN1775755A (en) | 2006-05-24 |
| CN100361976C CN100361976C (en) | 2008-01-16 |
Family
ID=36765495
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101229540A Expired - Fee Related CN100361976C (en) | 2005-12-06 | 2005-12-06 | Method for preparing raw material of pleuromutilin for use in tiamulin synthesizing process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100361976C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676257A (en) * | 2008-09-17 | 2010-03-24 | 大英九合生物化工股份有限公司 | Method for fermenting, extracting and preparing high purity pleuromutilin raw material |
| CN101319234B (en) * | 2008-07-04 | 2011-02-16 | 江苏赛奥生化有限公司 | Fermentation method for pleuromulin |
| CN102351698A (en) * | 2011-08-15 | 2012-02-15 | 上海华震科技有限公司 | Adsorption chromatograph based method for recovering pleuromutilin from crystallization mother liquor |
| CN102633641A (en) * | 2012-03-21 | 2012-08-15 | 宁夏泰瑞制药股份有限公司 | Method for extracting pleuromutilin from tiamulin fermentation liquor |
| CN102675172A (en) * | 2012-04-27 | 2012-09-19 | 宁夏泰瑞制药股份有限公司 | Preparation method of tiamulin base |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3949079A (en) * | 1964-04-17 | 1976-04-06 | Biochemie Ges.M.B.H. | Antibiotic derivatives |
| AT301752B (en) * | 1969-07-21 | 1972-09-25 | Biochemie Gmbh | Process for the preparation of new pleuromutilin derivatives |
-
2005
- 2005-12-06 CN CNB2005101229540A patent/CN100361976C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319234B (en) * | 2008-07-04 | 2011-02-16 | 江苏赛奥生化有限公司 | Fermentation method for pleuromulin |
| CN101676257A (en) * | 2008-09-17 | 2010-03-24 | 大英九合生物化工股份有限公司 | Method for fermenting, extracting and preparing high purity pleuromutilin raw material |
| CN102351698A (en) * | 2011-08-15 | 2012-02-15 | 上海华震科技有限公司 | Adsorption chromatograph based method for recovering pleuromutilin from crystallization mother liquor |
| CN102633641A (en) * | 2012-03-21 | 2012-08-15 | 宁夏泰瑞制药股份有限公司 | Method for extracting pleuromutilin from tiamulin fermentation liquor |
| CN102675172A (en) * | 2012-04-27 | 2012-09-19 | 宁夏泰瑞制药股份有限公司 | Preparation method of tiamulin base |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100361976C (en) | 2008-01-16 |
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Effective date of registration: 20190404 Address after: 310000 Room F, 9/F, Building A, Paradise Software Park, No. 3 Xidoumen Road, Xihu District, Hangzhou City, Zhejiang Province Patentee after: ZHEJIANG ZHEJIANG UNIVERSITY SUNSHINE TECHNOLOGY CO.,LTD. Address before: 226005 No. 98 Yuejiang Road, Nantong City, Jiangsu Province Patentee before: JIANGSU SEL BIOCHEMISTRY Co.,Ltd. |
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Effective date of registration: 20210825 Address after: 310000 block a, 9 / F, building a, Paradise Software Park, No. 3, xidoumen Road, Xihu District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou Shangni Biotechnology Co.,Ltd. Address before: 310000 Room F, 9/F, Building A, Paradise Software Park, No. 3 Xidoumen Road, Xihu District, Hangzhou City, Zhejiang Province Patentee before: ZHEJIANG ZHEJIANG UNIVERSITY SUNSHINE TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20211105 Address after: 226000 Building 2, No. 128, Changhe Road, Nantong, Jiangsu Province Patentee after: JIANGSU SEL BIOCHEMISTRY Co.,Ltd. Address before: 310000 block a, 9 / F, building a, Paradise Software Park, No. 3, xidoumen Road, Xihu District, Hangzhou City, Zhejiang Province Patentee before: Hangzhou Shangni Biotechnology Co.,Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080116 |