CN105566217B - A kind of purification process of fleraxacin crude product - Google Patents
A kind of purification process of fleraxacin crude product Download PDFInfo
- Publication number
- CN105566217B CN105566217B CN201610096468.4A CN201610096468A CN105566217B CN 105566217 B CN105566217 B CN 105566217B CN 201610096468 A CN201610096468 A CN 201610096468A CN 105566217 B CN105566217 B CN 105566217B
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- CN
- China
- Prior art keywords
- fleraxacin
- resin
- purification
- crude product
- product
- 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.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/16—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D215/48—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen
- C07D215/54—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen attached in position 3
- C07D215/56—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen attached in position 3 with oxygen atoms in position 4
Abstract
The present invention provides a kind of purification process of fleraxacin crude product.The preparation method is the certain density dissolving with hydrochloric acid of fleraxacin crude product for being 98.5% by content first, then it is at the uniform velocity added in processed ion exchange column in advance, column is washed with distillation, resin is parsed with certain density ammonium hydroxide after to the outflow of dark colour efflux, parsing feed liquid is evaporated under reduced pressure until there is precipitating, the filtering of room temperature growing the grain, it is dried to obtain fleraxacin product after purification, fleraxacin product content after purification can achieve 99.9% or more, yield reaches 90% or more, the purification process simple process, it is at low cost, commercialized production easy to accomplish.
Description
Technical field
The present invention relates to the purification process of drug chemical, specifically, being a kind of purification process of fleraxacin crude product.
Background technique
Fleraxacin is third generation fluoquinolone antibiotics, and outstanding advantages are to remove long half time, reachable 9 ~ 13 h,
The vivo medicine concentration duration is long, treats all kinds of infection both at home and abroad with the medicine and has obtained good efficacy.Fleraxacin has anti-
The features such as bacterium spectrum is wide, and toxic side effect is small, therefore be clinically widely applied.
The fleraxacin country has many producers and is producing, and has many synthetic routes, and every route has feature.At present
The purity of fleraxacin material medicine is different in the market, and generally 98.5% or so, the purity for improving fleraxacin can have
Effect improves the interior quality of drug.
The principle of analog is adsorbed according to analog, general non-polar resin is suitable for the absorption nonpolarity from polar solvent to have
Machine substance, opposite polarity resin, which is suitable for from nonpolar solvent, adsorbs polar solute.Middle polarity adsorbs resin, not only can be from non-
Polar substances are adsorbed in aqueous medium, and apolar substance can be also adsorbed from polar solvent.According to fleraxacin design feature, use
The fleraxacin crude product that the content that macroreticular resin prepares producer is 98.5% is purified, the product after separating to resin
HPLC analysis is carried out, product purity reaches 99.9% or more after purification, and purifying yield reaches 90% or more, and the present invention is by fleraxacin
Crude product improves this problem of the purity of fleraxacin with macroporous resin purification, and obtains exciting result.
Summary of the invention
The object of the present invention is to provide a kind of purification process of fleraxacin crude product.The purification process simple process, cost
It is low, commercialized production easy to accomplish.
In order to achieve the above object, the invention adopts the following technical scheme:
Macroreticular resin is packed into ion exchange column, washs resin with dehydrated alcohol, washing terminates followed by use salt-free water
Wash resin, then use the salt acid elution resin of 2mol/L, finally with salt-free water washing resin, by content for 98.5% fluorine Luo Sha
Star crude product, which is added in certain density acid, to be dissolved, and is at the uniform velocity added in ion exchange column, sample after resin layer completely into using
Distillation washing column parses resin with certain density lye until dark colour efflux flows completely out resin, by parsing feed liquid decompression
Until being evaporated to appearance precipitating, the filtering of room temperature growing the grain is dried to obtain fleraxacin product after purification, fleraxacin after purification
Product content can achieve 99.9% or more, and yield reaches 90% or more.
The macroreticular resin is strong-acid type benzene macroreticular resin ethylene system.
The certain density lye is the ammonium hydroxide that content is 3%-9% concentration.
The purification process of fleraxacin crude product of the present invention, which is characterized in that comprise the steps of:
Strong-acid type benzene macroreticular resin ethylene system is packed into ion exchange column, washs resin with dehydrated alcohol, washing terminates
Followed by with salt-free water washing resin, then with the salt acid elution resin of 2mol/L it is by content finally with salt-free water washing resin
98.5% fleraxacin crude product, which is added in the hydrochloric acid of 20%-30% concentration, to be dissolved, and is at the uniform velocity added in ion exchange column, sample
It is parsed until dark colour efflux flows completely out resin with the ammonium hydroxide of 3%-9% concentration completely into after resin layer with distillation washing column
Parsing feed liquid is evaporated under reduced pressure until there is precipitating resin, and room temperature growing the grain filtering, the fleraxacin being dried to obtain after purification produces
Product, fleraxacin product content after purification can achieve 99.9% or more, and yield reaches 90% or more.
The preparation method is simple, at low cost, easy to accomplish to commercially produce.
Specific embodiment
Here is the embodiment of the present invention, and the embodiment described is used only to illustrate the present invention, and is not considered as
Limitation of the present invention.
Embodiment 1
Strong-acid type benzene macroreticular resin ethylene system is packed into ion exchange column, washs resin with dehydrated alcohol, washing terminates
Followed by with salt-free water washing resin, then with the salt acid elution resin of 2mol/L it is by content finally with salt-free water washing resin
98.5% fleraxacin crude product 4.0g, which is added in the hydrochloric acid of 27% concentration, to be dissolved, and is at the uniform velocity added in ion exchange column, sample
Column is washed with distillation completely into after resin layer, until dark colour efflux flows completely out resin, with the ammonium hydroxide analytic tree of 5% concentration
Parsing feed liquid is evaporated under reduced pressure until there is precipitating rouge, and the filtering of room temperature growing the grain is dried to obtain fleraxacin product after purification
3.6g, fleraxacin product content after purification are 99.9%, and yield reaches 90%.
Embodiment 2
Strong-acid type benzene macroreticular resin ethylene system is packed into ion exchange column, washs resin with dehydrated alcohol, washing terminates
Followed by with salt-free water washing resin, then with the salt acid elution resin of 2mol/L it is by content finally with salt-free water washing resin
98.6% fleraxacin crude product 50.0g, which is added in the hydrochloric acid of 27% concentration, to be dissolved, and is at the uniform velocity added in ion exchange column, sample
Column is washed with distillation completely into after resin layer, until dark colour efflux flows completely out resin, with the ammonium hydroxide analytic tree of 5% concentration
Parsing feed liquid is evaporated under reduced pressure until there is precipitating rouge, and the filtering of room temperature growing the grain is dried to obtain fleraxacin product after purification
46.3g, fleraxacin product content after purification are 99.93%, and yield reaches 92.6%.
The purification process of fleraxacin crude product provided by the present invention is described in detail above, it is used herein
A specific example illustrates the principle and implementation of the invention, and the above embodiments are only used to help understand originally
The method and its core concept of invention；At the same time, for those skilled in the art, according to the thought of the present invention, specific
There will be changes in embodiment and application range, in conclusion the content of the present specification should not be construed as to of the invention
Limitation.
Claims (1)
1. a kind of purification process of fleraxacin crude product, which is characterized in that comprise the steps of: strong-acid type polystyrene macropore
Resin is packed into ion exchange column, wash resin with dehydrated alcohol, and washing end is followed by with salt-free water washing resin, then uses
The salt acid elution resin of 2mol/L adds the fleraxacin crude product 50.0g that content is 98.6% finally with salt-free water washing resin
Enter into the hydrochloric acid of 27% concentration and dissolve, be at the uniform velocity added in ion exchange column, sample is washed completely into after resin layer with distillation
Column parses resin with the ammonium hydroxide of 5% concentration, parsing feed liquid is evaporated under reduced pressure to appearance until dark colour efflux flows completely out resin
Until precipitating, the filtering of room temperature growing the grain is dried to obtain fleraxacin product 46.3g after purification, fleraxacin product after purification
Content is 99.93%, and yield reaches 92.6%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610096468.4A CN105566217B (en) | 2016-02-23 | 2016-02-23 | A kind of purification process of fleraxacin crude product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610096468.4A CN105566217B (en) | 2016-02-23 | 2016-02-23 | A kind of purification process of fleraxacin crude product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105566217A CN105566217A (en) | 2016-05-11 |
| CN105566217B true CN105566217B (en) | 2019-03-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610096468.4A Expired - Fee Related CN105566217B (en) | 2016-02-23 | 2016-02-23 | A kind of purification process of fleraxacin crude product |
Country Status (1)
| Country | Link |
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| CN (1) | CN105566217B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633639A (en) * | 2009-08-26 | 2010-01-27 | 海南美大制药有限公司 | High-purity fleroxacin compound |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PT775114E (en) * | 1994-08-02 | 2000-09-29 | Procter & Gamble | PROCESS FOR PRODUCING ANTIMICROBIAL COMPOUNDS |
-
2016
- 2016-02-23 CN CN201610096468.4A patent/CN105566217B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633639A (en) * | 2009-08-26 | 2010-01-27 | 海南美大制药有限公司 | High-purity fleroxacin compound |
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| Publication number | Publication date |
|---|---|
| CN105566217A (en) | 2016-05-11 |
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Granted publication date: 20190301 Termination date: 20200223 |