CN107382754A - A kind of quick high-efficiency synthesis method for preparing mefenamic acid - Google Patents
A kind of quick high-efficiency synthesis method for preparing mefenamic acid Download PDFInfo
- Publication number
- CN107382754A CN107382754A CN201710556033.8A CN201710556033A CN107382754A CN 107382754 A CN107382754 A CN 107382754A CN 201710556033 A CN201710556033 A CN 201710556033A CN 107382754 A CN107382754 A CN 107382754A
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- China
- Prior art keywords
- acid
- mefenamic acid
- preparing
- synthesis method
- mefenamic
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
- C07C227/06—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid
- C07C227/08—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid by reaction of ammonia or amines with acids containing functional groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
- C07C227/42—Crystallisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of quick high-efficiency synthesis method for preparing mefenamic acid, including：Step 1: following material is added into the container with agitating function：2,3 dimethylanilines, 0-chloro-benzoic acid, sodium acetate, catalyst and water, it is heated to 100~130 DEG C so that 2,3 dimethylanilines and 0-chloro-benzoic acid react to obtain reactant mixture；Step 2: making the reactant mixture in the step 1 naturally cool to room temperature, PH to 2.5 is adjusted, is filtrated to get mefenamic acid crude product；Step 3: the mefenamic acid crude product that the step 2 is prepared is washed with detergent, the detergent is the acid solution of PH2~3；Step 4: adding acetic acid recrystallization into the mefenamic acid crude product after step 3 washing, filtering, the mefenamic acid is dried to obtain.This method not only prepares that elapsed time is short, and the cost purity being prepared is high.
Description
Technical field
The present invention relates to technical field prepared by mefenamic acid, more particularly to a kind of quick side of efficiently synthesizing for preparing mefenamic acid
Method.
Background technology
Mefenamic acid is called the wet pain of Piao, is a kind of nonsteroid anti-inflammatory analgestic, for clinical time for a long time.First once
It is used to treat rheumatoid arthritis, osteoarthritis etc. afterwards, its curative effect and side effect and some other nonsteroid anti-inflammatory drugs phase
Seemingly.
In the prior art, the preparation method of mefenamic acid is typically more cumbersome, and time-consuming, and it is higher to prepare cost.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of quick side of efficiently synthesizing for preparing mefenamic acid
Method.This method not only prepares that elapsed time is short, and the cost purity being prepared is high.
The present invention proposes a kind of quick high-efficiency synthesis method for preparing mefenamic acid, including：
Step 1: following material is added into the container with agitating function：2,3- dimethylanilines, 0-chloro-benzoic acid, acetic acid
Sodium, catalyst and water, it is heated to 100~130 DEG C so that 2,3- dimethylanilines and 0-chloro-benzoic acid react to obtain reaction mixing
Thing；
Step 2: making the reactant mixture in the step 1 naturally cool to room temperature, PH to 2.5 is adjusted, first is filtrated to get and goes out
Acid crude；
Step 3: the mefenamic acid crude product that the step 2 is prepared is washed with detergent, the detergent is PH2~3
Acid solution；
Step 4: adding acetic acid recrystallization into the mefenamic acid crude product after step 3 washing, filtering, the first is dried to obtain
Fenamic acid.
In further technical scheme, the reaction time is 20h~30h in the step 1.
In further technical scheme, in the step 3, detergent temperature is previously heated to 30~35 DEG C during washing.
In further technical scheme, in the step 3, the acid solution is hydrochloric acid solution.
In further technical scheme, in the step 1, the catalyst is copper acetate.
The present invention compared with prior art, has the advantages that：
The present invention carries out quick wash using detergent to mefenamic acid crude product, improves product purity.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment 1
Following material is added into the container with agitating function：2,3- dimethylanilines, 0-chloro-benzoic acid, sodium acetate, acetic acid
Copper and water, it is heated to 130 DEG C so that 2,3- dimethylanilines and 0-chloro-benzoic acid react to obtain reactant mixture, reaction time
For 10h；Reactant mixture naturally cools to room temperature, adjusts PH to 2.5, is filtrated to get mefenamic acid crude product；Mefenamic acid crude product is with washing
Agent washing is washed, the detergent is PH2 acid solution, and detergent temperature is previously heated to 30~35 DEG C；First after washing
Acetic acid recrystallization is added in fenamic acid crude product, filtering, is dried to obtain mefenamic acid product.
Embodiment 2
Following material is added into the container with agitating function：2,3- dimethylanilines, 0-chloro-benzoic acid, sodium acetate, acetic acid
Copper and water, are heated to 100 so that 2,3- dimethylanilines and 0-chloro-benzoic acid react to obtain reactant mixture, and the reaction time is
25h；；Reactant mixture naturally cools to room temperature, adjusts PH to 2.5, is filtrated to get mefenamic acid crude product；Mefenamic acid crude product washs
Agent is washed, and the detergent is PH3 acid solution, and detergent temperature is previously heated to 30~35 DEG C；First after washing is gone out
Acetic acid recrystallization is added in acid crude, filtering, is dried to obtain mefenamic acid product.
Embodiment 3
Following material is added into the container with agitating function：2,3- dimethylanilines, 0-chloro-benzoic acid, sodium acetate, acetic acid
Copper and water, it is heated to 110 DEG C so that 2,3- dimethylanilines and 0-chloro-benzoic acid react to obtain reactant mixture, reaction time
For 30h；；Reactant mixture naturally cools to room temperature, adjusts PH to 2.5, is filtrated to get mefenamic acid crude product；Mefenamic acid crude product is with washing
Agent washing is washed, the detergent is PH2 hydrochloric acid solution, and detergent temperature is previously heated to 30~35 DEG C；After washing
Acetic acid recrystallization is added in mefenamic acid crude product, filtering, is dried to obtain mefenamic acid product.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (5)
- A kind of 1. quick high-efficiency synthesis method for preparing mefenamic acid, it is characterised in that including：Step 1: following material is added into the container with agitating function：2,3- dimethylanilines, 0-chloro-benzoic acid, acetic acid Sodium, catalyst and water, it is heated to 100~130 DEG C so that 2,3- dimethylanilines and 0-chloro-benzoic acid react to obtain reaction mixing Thing；Step 2: making the reactant mixture in the step 1 naturally cool to room temperature, PH to 2.5 is adjusted, first is filtrated to get and goes out Acid crude；Step 3: the mefenamic acid crude product that the step 2 is prepared is washed with detergent, the detergent is PH2~3 Acid solution；Step 4: adding acetic acid recrystallization into the mefenamic acid crude product after step 3 washing, filtering, the first is dried to obtain Fenamic acid.
- A kind of 2. quick high-efficiency synthesis method for preparing mefenamic acid according to claim 1, it is characterised in that the step The reaction time is 20h~30h in one.
- A kind of 3. quick high-efficiency synthesis method for preparing mefenamic acid according to claim 1, it is characterised in that the step In three, detergent temperature is previously heated to 30~35 DEG C during washing.
- A kind of 4. quick high-efficiency synthesis method for preparing mefenamic acid according to claim 1, it is characterised in that the step In three, the acid solution is hydrochloric acid solution.
- A kind of 5. quick high-efficiency synthesis method for preparing mefenamic acid according to claim 1, it is characterised in that the step In one, the catalyst is copper acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710556033.8A CN107382754A (en) | 2017-07-10 | 2017-07-10 | A kind of quick high-efficiency synthesis method for preparing mefenamic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710556033.8A CN107382754A (en) | 2017-07-10 | 2017-07-10 | A kind of quick high-efficiency synthesis method for preparing mefenamic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107382754A true CN107382754A (en) | 2017-11-24 |
Family
ID=60333858
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710556033.8A Pending CN107382754A (en) | 2017-07-10 | 2017-07-10 | A kind of quick high-efficiency synthesis method for preparing mefenamic acid |
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| CN (1) | CN107382754A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552199A (en) * | 2020-12-08 | 2021-03-26 | 北京金城泰尔制药有限公司沧州分公司 | Preparation method of large-crystal high-bulk-density mefenamic acid |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475505A (en) * | 2009-02-09 | 2009-07-08 | 宝鸡天新医药化工有限公司 | Process for preparing mefenamic acid |
| CN101704761A (en) * | 2009-10-23 | 2010-05-12 | 宁波斯迈克制药有限公司 | Synthesis method of mefenamic acid |
| CN102344384A (en) * | 2011-09-02 | 2012-02-08 | 德州博诚制药有限公司 | Production method of mefenamic acid |
| CN105949075A (en) * | 2016-06-24 | 2016-09-21 | 江苏倍合德化工有限公司 | Synthesis method of mefenamic acid |
| CN106380414A (en) * | 2016-08-30 | 2017-02-08 | 西安利君精华药业有限责任公司 | Mefenamic acid and synthesis technology thereof |
-
2017
- 2017-07-10 CN CN201710556033.8A patent/CN107382754A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475505A (en) * | 2009-02-09 | 2009-07-08 | 宝鸡天新医药化工有限公司 | Process for preparing mefenamic acid |
| CN101704761A (en) * | 2009-10-23 | 2010-05-12 | 宁波斯迈克制药有限公司 | Synthesis method of mefenamic acid |
| CN102344384A (en) * | 2011-09-02 | 2012-02-08 | 德州博诚制药有限公司 | Production method of mefenamic acid |
| CN105949075A (en) * | 2016-06-24 | 2016-09-21 | 江苏倍合德化工有限公司 | Synthesis method of mefenamic acid |
| CN106380414A (en) * | 2016-08-30 | 2017-02-08 | 西安利君精华药业有限责任公司 | Mefenamic acid and synthesis technology thereof |
Non-Patent Citations (1)
| Title |
|---|
| GIRISHA, HANAKERE R.等: "A simple and environmentally friendly method for the synthesis of N-phenylanthranilic acid derivatives", 《JOURNAL OF CHEMICAL RESEARCH》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552199A (en) * | 2020-12-08 | 2021-03-26 | 北京金城泰尔制药有限公司沧州分公司 | Preparation method of large-crystal high-bulk-density mefenamic acid |
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