CN107936068A - A kind of net process for purification of Ai Gelie - Google Patents
A kind of net process for purification of Ai Gelie Download PDFInfo
- Publication number
- CN107936068A CN107936068A CN201711317400.5A CN201711317400A CN107936068A CN 107936068 A CN107936068 A CN 107936068A CN 201711317400 A CN201711317400 A CN 201711317400A CN 107936068 A CN107936068 A CN 107936068A
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- CN
- China
- Prior art keywords
- gelie
- ethanol
- net
- purification
- volume
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- 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
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H9/00—Compounds containing a hetero ring sharing at least two hetero atoms with a saccharide radical
- C07H9/02—Compounds containing a hetero ring sharing at least two hetero atoms with a saccharide radical the hetero ring containing only oxygen as ring hetero atoms
- C07H9/04—Cyclic acetals
Abstract
The present invention relates to a kind of net process for purification of Ai Gelie, belong to bulk pharmaceutical chemicals preparing technical field.The technical scheme is that：The net crude products of Ai Gelie are dissolved in 95% ethanol first；The activated carbon added thereto, is stirred, filtering；Filtrate is cooled to 72 DEG C, and the mixed solution of ethanol acetone is slowly added dropwise thereto, there is white solid precipitation, continue stirring 58 it is small when；Filtering, filter cake are washed with 95% ethanol solution；30 DEG C of vacuum drying of filter cake.The present invention provides a kind of method that refined Ai Gelie is net, and a kind of bulk pharmaceutical chemicals of high quality can be provided for preparation.
Description
Technical field
The present invention relates to a kind of net process for purification of Ai Gelie, belong to bulk pharmaceutical chemicals preparing technical field.
Background technology
Diabetes are one group of metabolic diseases characterized by hyperglycaemia.Counted according to International Diabetes Federation, 2014 complete
Ball diabetic is up to 3.87 hundred million people, it is contemplated that is up to 5.92 hundred million people within 2035.Type ii diabetes are the most common shape of diabetes
Formula, accounts for the 90% of diabetic.
Diabetes can cause the various tissues of human body, especially eye, kidney, heart, blood vessel, the chronic lesion of nerve, function
Obstacle.Once as diabetic, it is necessary to take medicine throughout one's life.Diabetes not only influence the quality of life of patient, it is also possible to lead
Cause the shortening in service life.
Ai Gelie is net, English name Ertugliflozin, and chemistry is entitled：1,6- dehydrations -1-C- [the chloro- 3- of 4-
[(4- ethoxyl phenenyls) methyl] phenyl] -5-C- (hydroxymethyl)-BETA-L- idoses, mode of being used as medicine is Ai Gelie net-burnt
Glutamic acid compound, Mo Shadong (Merck) and Pfizer (Pfizer) company joint research and development, submit listing in March, 2017 to FDA
Application.Ai Gelie belongs to small dimension preparation only, commercially available to have 5mg and 15mg；Ai Gelie is only not soluble in water, and complicated.
It will be apparent to one skilled in the art that the presence of impurity can influence the effect of medicine, some can even produce malicious secondary work
With.Process for purification document net no Ai Gelie discloses in the prior art.
The content of the invention
The object of the present invention is to provide a kind of net process for purification of Ai Gelie, while providing quality raw materials medicine for preparation, drop
Low industrially prepared cost.
Technical solution：
The technical scheme is that：
A kind of net process for purification of Ai Gelie, comprises the following steps：
The net crude products of Ai Gelie are dissolved in 95% ethanol by the first step；
The preferable technical solution of this step, the concentration of prepared solution is 15-22%（Quality percent by volume）.
Second step at room temperature, the net crude product amount 7-10% of first step Ai Gelie is added into first step filtrate（Percentage by weight）
Activated carbon, stirring 1.2-2 it is small when, filtering；
Under the stirring of 3rd step, second step filtrate is cooled to -7-2 DEG C, the mixed solution of ethanol-acetone is slowly added dropwise thereto,
The volume that mixed solution is added dropwise is the 35-55% of first step volume；Have white solid precipitation, continue stir 5-8 it is small when；It is described mixed
In bonding solvent, the volume ratio of ethanol-acetone is 5:1.8-3.2.
The preferable technical solution of this step, the speed that ethanol-acetone mixed solution is added dropwise are 1.1-2.2ml/ minutes.
4th step filters, and filter cake is washed with 95% ethanol solution；
The preferable technical solution of this step, filter cake are washed 3 times with 95% ethanol solution, and each dosage is first step quantity of solvent
8-10%。
5th step filter cake is spread out, 30 DEG C of vacuum drying.
Useful achievement：The present invention provides the net purity of Ai Gelie prepared by a kind of method that refined Ai Gelie is net, this method
More than 99.88%, a kind of bulk pharmaceutical chemicals of high quality are provided for preparation.
The embodiment embodiment of the present invention is prepared with the net crude products of Ai Gelie by the prior art, its is pure for high performance liquid chromatography detection
Spend for 96.48%.
Embodiment 1,
The net crude products of 15g Ai Gelie are dissolved in 95% ethanol of 100ml by the first step；
Second step at room temperature, 1.05g activated carbons is added into first step filtrate, when stirring 1.2 is small, filtering；
Under the stirring of 3rd step, second step filtrate is cooled to -7 DEG C, the mixing that 35ml ethanol-acetones are slowly added dropwise thereto is molten
Liquid, the speed that ethanol-acetone mixed solution is added dropwise are 1.1ml/ minutes；Have white solid precipitation, continue stirring 5 it is small when；It is described
In the mixed solvent, the volume ratio of ethanol-acetone is 5:1.8.
4th step filters, and filter cake is washed 3 times with 95% ethanol solution, and each dosage is 8ml；
5th step filter cake is spread out, 30 DEG C of vacuum drying.Products obtained therefrom high performance liquid chromatography detection purity is 99.89%, yield
92.87%。
Embodiment 2,
The net crude products of 22g Ai Gelie are dissolved in 95% ethanol of 100ml by the first step；
Second step at room temperature, 2.2g activated carbons is added into first step filtrate, when stirring 2 is small, filtering；
Under the stirring of 3rd step, second step filtrate is cooled to 2 DEG C, the mixing that 55ml ethanol-acetones are slowly added dropwise thereto is molten
Liquid, be added dropwise ethanol-acetone mixed solution speed be 2.2ml/ minute, have white solid precipitation, continue stir 8 it is small when；It is described
In the mixed solvent, the volume ratio of ethanol-acetone is 5:3.2.
4th step filters, and filter cake is washed 3 times with 95% ethanol solution, and each dosage is 10ml；
5th step filter cake is spread out, 30 DEG C of vacuum drying.Products obtained therefrom high performance liquid chromatography detection purity is 99.95%, yield
93.24%。
Embodiment 3,
The net crude products of 20g Ai Gelie are dissolved in 95% ethanol by the first step；
Second step at room temperature, 1.9g activated carbons is added into first step filtrate, when stirring 1.7 is small, filtering；
Under the stirring of 3rd step, second step filtrate is cooled to -3 DEG C, slowly drop, the mixing of 48ml ethanol-acetones are molten thereto
Liquid, be added dropwise ethanol-acetone mixed solution speed be 1.8l/ minute, have white solid precipitation, continue stir 7 it is small when；It is described mixed
In bonding solvent, the volume ratio of ethanol-acetone is 5:2.6.
4th step filters, and filter cake washs washing 3 times with 95% ethanol solution, and each dosage is 9ml；
5th step filter cake is spread out, 30 DEG C of vacuum drying.Products obtained therefrom high performance liquid chromatography detection purity is 99.98%, yield
93.17%。
Claims (5)
1. a kind of net process for purification of Ai Gelie, it is characterised in that comprise the following steps：
The net crude products of Ai Gelie are dissolved in 95% ethanol by the first step；
Second step at room temperature, the net crude product amount 7-10% of first step Ai Gelie is added into first step filtrate（Percentage by weight）Work
Property charcoal, stirring 1.2-2 it is small when, filtering；
Under the stirring of 3rd step, second step filtrate is cooled to -7-2 DEG C, the mixed solution of ethanol-acetone is slowly added dropwise thereto,
The volume that mixed solution is added dropwise is the 35-55% of first step volume；Have white solid precipitation, continue stir 5-8 it is small when；It is described mixed
In bonding solvent, the volume ratio of ethanol-acetone is 5:1.8-3.2；
4th step filters, and filter cake is washed with 95% ethanol solution；
5th step filter cake is spread out, 30 DEG C of vacuum drying.
2. according to the net process for purification of Ai Gelie described in claim 1, it is characterised in that the quality volume of solution prepared by the first step
Percent concentration is 15-22%.
3. according to the net process for purification of Ai Gelie described in claim 1, it is characterised in that it is molten that ethanol-acetone mixing is added dropwise in the 3rd step
The speed of liquid is 1.1-2.2ml/ minutes.
4. according to the net process for purification of Ai Gelie described in claim 1, it is characterised in that it is molten that ethanol-acetone mixing is added dropwise in the 3rd step
The volume of liquid is the 40-50% of first step volume.
5. according to the net process for purification of Ai Gelie described in claim 1, it is characterised in that the 4th step filter cake with 95% ethanol solution
Washing 3 times, each dosage are the 8-10% of first step quantity of solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711317400.5A CN107936068A (en) | 2017-12-12 | 2017-12-12 | A kind of net process for purification of Ai Gelie |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711317400.5A CN107936068A (en) | 2017-12-12 | 2017-12-12 | A kind of net process for purification of Ai Gelie |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107936068A true CN107936068A (en) | 2018-04-20 |
Family
ID=61942669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711317400.5A Withdrawn CN107936068A (en) | 2017-12-12 | 2017-12-12 | A kind of net process for purification of Ai Gelie |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107936068A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320463A (en) * | 2018-10-07 | 2019-02-12 | 威海贯标信息科技有限公司 | A kind of purification process of small grain size ambrisentan |
| CN110655511A (en) * | 2019-05-31 | 2020-01-07 | 北京莱瑞森医药科技有限公司 | Preparation and refining method of high-purity empagliflozin |
-
2017
- 2017-12-12 CN CN201711317400.5A patent/CN107936068A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320463A (en) * | 2018-10-07 | 2019-02-12 | 威海贯标信息科技有限公司 | A kind of purification process of small grain size ambrisentan |
| CN110655511A (en) * | 2019-05-31 | 2020-01-07 | 北京莱瑞森医药科技有限公司 | Preparation and refining method of high-purity empagliflozin |
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| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180420 |
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| WW01 | Invention patent application withdrawn after publication |