CN107793346A - A kind of process for purification of arbidol HCl - Google Patents
A kind of process for purification of arbidol HCl Download PDFInfo
- Publication number
- CN107793346A CN107793346A CN201711188073.8A CN201711188073A CN107793346A CN 107793346 A CN107793346 A CN 107793346A CN 201711188073 A CN201711188073 A CN 201711188073A CN 107793346 A CN107793346 A CN 107793346A
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- ethanol water
- purification
- volume
- arbidol hcl
- percent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/30—Indoles; Hydrogenated indoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to carbon atoms of the hetero ring
- C07D209/42—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of preparation method of Abiduoer, belong to bulk drug preparing technical field.Technical scheme comprises the following steps：Arbidol HCl is dissolved in tetrahydrofuran solution, stirs lower dissolving, filtering；Under stirring, ethanol water is slowly added dropwise into first step filtrate；Slow cooling stirs lower addition first step quantity of solvent 10 18% to 5 DEG C 0 DEG C（Percent by volume）Water continue stirring 12 hours；Filtering, filter cake concentration is 50 65%（Percent by volume）The ethanol water of scope washs 3 times；Spread filter cake out, in 45 DEG C of vacuum drying, obtain high-purity hydrochloric acid Abiduoer.The invention provides a kind of simple and easy arbidol HCl process for refining.
Description
Technical field
The present invention relates to a kind of preparation method of Abiduoer, belong to bulk drug preparing technical field.
Background technology
Abiduoer, chemical name：The bromo- 4- of 6-（Dimethylamino methyl）- 5- hydroxyl -1- methyl -2-（Benzene sulfidomethyl）-
1H- indole -3-carboxylic acid's carbethoxy hydrochlorides, form of being used as medicine are the monohydrate of Abiduoer.Abiduoer is a kind of antiviral agent
Thing, developed by former Soviet Union's pharmaceutical chemistry research center, principal indication is A classes, popular sexy caused by B parainfluenza virus
Emit, while may also have antiviral activity to some other respiratory virus infection.Because its adverse events incidence is about
6.2%, it is mainly shown as that nausea, diarrhoea, dizzy and serum transaminase increase, have impact on clinical expansion utilization.
Because its structure is complex, and preparation process is grown, it is not easy to and it is refined, the popularization of its industrialized production is have impact on,
The document of the not refined Abiduoer of prior art discloses.
Content of the invention goal of the invention：A kind of process for purification of Abiduoer is provided, quality raw materials medicine is provided for clinic, reduces
Adverse reaction rate.
Technical scheme：
The technical scheme is that：A kind of process for purification of arbidol HCl, comprises the following steps：
First step arbidol HCl is dissolved in tetrahydrofuran solution, stirs lower dissolving, filtering；
This step resulting solution concentration is in 9-18%（Quality percent by volume）Scope.
Under second step stirring, ethanol water is slowly added dropwise into first step filtrate；The concentration of the ethanol water exists
50-65%（Percent by volume）Scope；Dropwise addition flow velocity is 0.45ml -0.70ml per minute；
The preferable scheme of this step, the concentration of the ethanol water is in 56-62%（Percent by volume）Scope is preferably added dropwise
The amount of ethanol water is the 30-50% of first step quantity of solvent；
The preferable scheme of this step, the amount that ethanol water is added dropwise are the 36-43%. of first step quantity of solvent
Second step solution slow cooling to -5 DEG C -0 DEG C, is stirred lower addition first step quantity of solvent 10-18% by the 3rd step（Volume hundred
Divide ratio）Water, have white solid precipitation, continue stir 1-2 hours；
The preferable technical scheme of this step, the amount for adding water are the 12-15% of first step quantity of solvent.
4th step filters, and filter cake concentration is in 50-65%（Percent by volume）The ethanol water washing of scope 3 times, often
Secondary ethanol water 15-25ml.
5th step spreads filter cake out, in 45 DEG C of vacuum drying, obtains high-purity hydrochloric acid Abiduoer.
Useful achievement：The invention provides a kind of simple and easy arbidol HCl process for refining, the technology of the present invention side
Case products obtained therefrom purity is up to more than 99.95%.High-quality bulk drug is provided for arbidol HCl preparation, is made for improving
The quality of agent has positive meaning.
Abiduoer crude product used in embodiment embodiment of the present invention use is prepared by prior art, and high performance liquid chromatography is surveyed
Purity is determined for 96.79%.
Embodiment 1,9g arbidol HCls are dissolved in 100ml tetrahydrofuran solutions, stirring and dissolving, filtering；To filtrate
In 30ml 50% ethanol water is slowly added dropwise, dropwise addition flow velocity is 0.45ml per minute；Solution slow cooling is to -5 DEG C, stirring
Lower addition 10ml water, there is white solid precipitation, continues stirring 1 hour；Filtering, filter cake concentration is 50%（Percent by volume）Model
The ethanol water enclosed washs 3 times, uses ethanol water 15ml every time.Spread filter cake out, in 45 DEG C of vacuum drying, obtain hydrochloric acid Ah ratio
Duo Er.Yield 93.01%, high effective liquid chromatography for measuring purity are 99.97%.
Embodiment 2,
18g arbidol HCls are dissolved in 100ml tetrahydrofuran solutions, stirring and dissolving, filtering；It is slowly added dropwise into filtrate
50ml 65% ethanol water, dropwise addition flow velocity are 0.7ml per minute；Solution slow cooling stirs lower addition 18ml to 0 DEG C
Water, there is white solid precipitation, continue stirring 1 hour；Filtering, filter cake concentration is 65%（Percent by volume）The ethanol water of scope
Solution washs 3 times, uses ethanol water 25ml every time.Spread filter cake out, in 45 DEG C of vacuum drying, obtain arbidol HCl.Yield
93.38%, high effective liquid chromatography for measuring purity is 99.99%.
Embodiment 3,15g arbidol HCls are dissolved in 100ml tetrahydrofuran solutions, stirring and dissolving, filtering；To filter
40ml 60% ethanol water is slowly added dropwise in liquid, dropwise addition flow velocity is 0.6ml per minute；Solution slow cooling stirs to -2 DEG C
Lower addition 14ml water is mixed, there is white solid precipitation, continues stirring 1 hour；Filtering, filter cake concentration is 60%（Percent by volume）
The ethanol water of scope washs 3 times, uses ethanol water 20ml every time.Spread filter cake out, in 45 DEG C of vacuum drying, obtain hydrochloric acid Ah
Compare Duo Er.Yield 93.30%, high effective liquid chromatography for measuring purity are 100.09%.
Claims (6)
1. a kind of process for purification of arbidol HCl, it is characterised in that comprise the following steps：
First step arbidol HCl is dissolved in tetrahydrofuran solution, stirs lower dissolving, filtering；
Under second step stirring, ethanol water is slowly added dropwise into first step filtrate, the concentration of the ethanol water is in 50-
65%（Percent by volume）Scope；Dropwise addition flow velocity is 0.45ml -0.70ml per minute；
Second step solution slow cooling to -5 DEG C -0 DEG C, is stirred lower addition first step quantity of solvent 10-18% by the 3rd step（Volume hundred
Divide ratio）Water, have white solid precipitation, continue stir 1-2 hours；
4th step filters, and filter cake concentration is in 50-65%（Percent by volume）The ethanol water of scope washs 3 times, uses every time
Ethanol water 15-25ml；
5th step spreads filter cake out, in 45 DEG C of vacuum drying, obtains high-purity hydrochloric acid Abiduoer.
2. according to the process for purification of claim 1 arbidol HCl, it is characterised in that the quality volume of first step resulting solution
Percent concentration is in 9-18% scopes.
3. according to the process for purification of claim 1 arbidol HCl, it is characterised in that the amount of ethanol water is added dropwise in second step
It is the 30-50% of first step quantity of solvent.
4. according to the process for purification of claim 1 arbidol HCl, it is characterised in that ethanol water described in second step it is dense
Degree is in 56-62%（Percent by volume）Scope.
5. according to the process for purification of claim 1 arbidol HCl, it is characterised in that the amount of ethanol water is added dropwise in second step
It is the 36-43% of first step quantity of solvent.
6. according to the process for purification of claim 1 arbidol HCl, it is characterised in that the amount that the 3rd step adds water is the first step
The 12-15% of quantity of solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711188073.8A CN107793346A (en) | 2017-11-24 | 2017-11-24 | A kind of process for purification of arbidol HCl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711188073.8A CN107793346A (en) | 2017-11-24 | 2017-11-24 | A kind of process for purification of arbidol HCl |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107793346A true CN107793346A (en) | 2018-03-13 |
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ID=61536594
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711188073.8A Withdrawn CN107793346A (en) | 2017-11-24 | 2017-11-24 | A kind of process for purification of arbidol HCl |
Country Status (1)
| Country | Link |
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| CN (1) | CN107793346A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117586173A (en) * | 2023-11-29 | 2024-02-23 | 石家庄中硕制药有限公司 | Preparation method of arbidol |
-
2017
- 2017-11-24 CN CN201711188073.8A patent/CN107793346A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117586173A (en) * | 2023-11-29 | 2024-02-23 | 石家庄中硕制药有限公司 | Preparation method of arbidol |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180313 |
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| WW01 | Invention patent application withdrawn after publication |