CN101092352A - Method for refining o - benzoylbenzoic acid - Google Patents
Method for refining o - benzoylbenzoic acid Download PDFInfo
- Publication number
- CN101092352A CN101092352A CN 200710069579 CN200710069579A CN101092352A CN 101092352 A CN101092352 A CN 101092352A CN 200710069579 CN200710069579 CN 200710069579 CN 200710069579 A CN200710069579 A CN 200710069579A CN 101092352 A CN101092352 A CN 101092352A
- Authority
- CN
- China
- Prior art keywords
- purification
- benzoylbenzoic acid
- acid
- benzoylbenzoic
- souring agent
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
This invention provides a rapid and effective method for refining o-benzoylbenzoic acid. The method comprises: adding crude o-benzoylbenzoic acid (content = 95-98%) into water, heating to 50 deg.C, slowly dropping alkali solution, adding activated carbon, heating to 80-90 deg.C, keeping for 2h, vacuum-filtering, removing activated carbon, cooling the filtrate to room temperature, adjusting the pH value to 1 at 40 deg.C with acidifier, stirring for 0.5 h, vacuum-filtering, washing the filter cake with a small amount of water, and drying at 70-80 deg.C for 16 h to obtain white product with o-benzoylbenzoic acid content higher than 99% (measured by HPLC) and yield higher than 90%. The method is suitable for industrialization.
Description
Technical field
The present invention relates to a kind of process for purification of o-benzoylbenzoic acid, belong to the fine chemistry industry preparing technical field.
Background technology
O-benzoylbenzoic acid has the structure shown in general formula 1, is the important intermediate of synthetic preservative OBBM (methyl o-benzoylbenzoate), and in addition, o-benzoylbenzoic acid also is the important intermediate of synthetic medical material medicine Fenazoxine and nefopam.
General formula I
In the market the o-benzoylbenzoic acid of being sold basically content be the faint yellow crystalloid powder of 95%-98%.Existing o-benzoylbenzoic acid process for purification usually with organic solvents such as ethanol as solvent, recrystallization and getting, product content is lower than 99%, and used organic solvent smell is big, the organic detritus that stays pollutes big, and is unfavorable in environmental protection.
Summary of the invention
The objective of the invention is for a kind of process for purification of simple and direct o-benzoylbenzoic acid efficiently is provided, can make the content ratio of product be easier to reach more than 99%, can be by industrialization.
The present invention is the process for purification of o-benzoylbenzoic acid, in water, add o-benzoylbenzoic acid crude product (content is 95%-98%), be warmed up to about 50 ℃, then dripping alkali liquid slowly, drip and finish, add gac, be warmed up to 80 ℃～90 ℃, be incubated 2 hours, suction filtration while hot, remove gac, the filtrate cool to room temperature is being adjusted to pH=1 with souring agent with solution below 40 ℃, stir half an hour, suction filtration washes filter cake with water, and drying is 16 hours under 70 ℃～80 ℃ conditions, obtain the pure white product, greater than 99%, yield is higher than 90% to content (HPLC is a high performance liquid phase, down together).
More than invention, described alkali lye can be potassium hydroxide aqueous solution, ammonia soln, aqueous sodium hydroxide solution, also can be the aqueous solution of strong base-weak acid salt.
Described souring agent can be strong acid such as hydrochloric acid, sulfuric acid, is preferably hydrochloric acid.
The present invention compares with prior art, has following outstanding advantage and positively effect:
1, avoids conventional usefulness organic solvent purified method, reduced cost, improved the yield of product.
2, constant product quality ground is reached more than 99%, and can obtain lily product.
3, easy and simple to handle efficient, can be used as industrialized preparing process.
4, organic solvent-free smell, no organic detritus is beneficial to environmental protection, is a kind of process for cleanly preparing.
Embodiment
Embodiment 1
In the four-hole bottle of 2000ml, the water that adds 800ml, the o-benzoylbenzoic acid crude product (content is 95%-98%) that adds 100g then, be warmed up to about 50 ℃, slowly drip 40% potassium hydroxide solution of 80ml then, drip and finish, add the 5g gac, be warmed up to 80 ℃～90 ℃, be incubated 2 hours, suction filtration is removed gac while hot, the filtrate cool to room temperature, at the sulfuric acid with 40% below 40 ℃ solution is adjusted to pH=1, stirs half an hour, suction filtration, a spot of water washing filter cake, drying is 16 hours under 70 ℃～80 ℃ conditions.Obtain the pure white product of 92.5g, content (HPLC) 99.21%, 128.1 ℃～129.5 ℃ of fusing points, yield 92.5%.
Embodiment 2
In the four-hole bottle of 2000ml, the water that adds 800ml, the o-benzoylbenzoic acid crude product (content is 95%-98%) that adds 100g then, be warmed up to about 50 ℃, slowly drip 40% sodium hydroxide solution of 80ml then, drip and finish, add the 5g gac, be warmed up to 80 ℃～90 ℃, be incubated 2 hours, suction filtration is removed gac while hot, the filtrate cool to room temperature, at the sulfuric acid with 40% below 40 ℃ solution is adjusted to pH=1, stirs half an hour, suction filtration, a spot of water washing filter cake, drying is 16 hours under 70 ℃ ~ 80 ℃ conditions.Obtain the pure white product of 90.3g, content (HPLC) 99.30%, 127.5 ℃～128.3 ℃ of fusing points, yield 90.3%.
Embodiment 3
In the four-hole bottle of 2000ml, the water that adds 800ml, the o-benzoylbenzoic acid crude product (content is 95%-98%) that adds 100g then, be warmed up to about 50 ℃, slowly drip the strong aqua (concentration is 17%-19%) of 180ml then, drip and finish, add the 5g gac, be warmed up to 80 ℃～90 ℃, be incubated 2 hours, suction filtration is removed gac while hot, the filtrate cool to room temperature, at the sulfuric acid with 40% below 40 ℃ solution is adjusted to pH=1, stirs half an hour, suction filtration, a spot of water washing filter cake, drying is 16 hours under 70 ℃ ~ 80 ℃ conditions.Obtain the pure white product of 91.6g, content (HPLC) 99.37%, 128.5 ℃～129.3 ℃ of fusing points, yield 91.6%.
Claims (9)
1, a kind of process for purification of o-benzoylbenzoic acid is characterized in that, described process for purification is, in water, add o-benzoylbenzoic acid crude product (content is 95%-98%), heat up first, then dripping alkali liquid slowly, drip to finish, add gac, heat up once more and be incubated, suction filtration while hot, remove gac, filtrate cooling back is with souring agent regulator solution pH=1 and stir suction filtration, wash filter cake with water, drying.
By the process for purification of the described o-benzoylbenzoic acid of claim 1, it is characterized in that 2, described intensification first is for being warmed up to 40 ℃-60 ℃.
3, by the process for purification of the described o-benzoylbenzoic acid of claim 1, it is characterized in that, describedly heat up once more and be incubated, be incubated 2 hours to being warmed up to 80 ℃～90 ℃.
4, press the process for purification of the described o-benzoylbenzoic acid of claim 1, it is characterized in that, described filtrate cooling back is the filtrate cool to room temperature with souring agent regulator solution pH=1 and stirring, with souring agent solution is being adjusted to pH=1 below 40 ℃, stirs half an hour.
By the process for purification of the described o-benzoylbenzoic acid of claim 1, it is characterized in that 5, described drying be a drying 16 hours under 70 ℃～80 ℃ conditions.
6, by the process for purification of any one described o-benzoylbenzoic acid in the claim 1 to 5, it is characterized in that described alkali lye is the aqueous solution of potassium hydroxide aqueous solution or ammonia soln or aqueous sodium hydroxide solution or strong base-weak acid salt.
7, by the process for purification of any one described o-benzoylbenzoic acid in the claim 1 to 5, it is characterized in that described souring agent is a strong acid.
8, by the process for purification of any one described o-benzoylbenzoic acid in the claim 1 to 5, it is characterized in that described souring agent is hydrochloric acid or sulfuric acid.
9, by the process for purification of any one described o-benzoylbenzoic acid in the claim 1 to 5, it is characterized in that described souring agent is a hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710069579 CN101092352A (en) | 2007-07-16 | 2007-07-16 | Method for refining o - benzoylbenzoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710069579 CN101092352A (en) | 2007-07-16 | 2007-07-16 | Method for refining o - benzoylbenzoic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101092352A true CN101092352A (en) | 2007-12-26 |
Family
ID=38990813
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710069579 Pending CN101092352A (en) | 2007-07-16 | 2007-07-16 | Method for refining o - benzoylbenzoic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101092352A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008187A (en) * | 2016-06-04 | 2016-10-12 | 江阴市长江化工有限公司 | Preparation method of synthetic anthraquinone |
| CN115521199A (en) * | 2021-12-31 | 2022-12-27 | 山东华夏神舟新材料有限公司 | Method and device for purifying benzophenone tetracarboxylic acid |
-
2007
- 2007-07-16 CN CN 200710069579 patent/CN101092352A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106008187A (en) * | 2016-06-04 | 2016-10-12 | 江阴市长江化工有限公司 | Preparation method of synthetic anthraquinone |
| CN106008187B (en) * | 2016-06-04 | 2018-08-28 | 江阴市长江化工有限公司 | A kind of preparation method of synthesis anthraquinone |
| CN115521199A (en) * | 2021-12-31 | 2022-12-27 | 山东华夏神舟新材料有限公司 | Method and device for purifying benzophenone tetracarboxylic acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104610161A (en) | Preparation method for telmisartan | |
| CN103102351B (en) | Refining method for preparing high-purity folic acid | |
| CN102964313B (en) | Synthetic method of febuxostat | |
| WO2023093677A1 (en) | Synthesis process for fatty acyl taurate | |
| CN105541633A (en) | open-chain chiral crown ether containing ent-Bayesian skeleton and preparation and application thereof | |
| CN1321121C (en) | Preparation and post-treatment method of levofloxacin | |
| CN109503568B (en) | Preparation method of dasatinib | |
| CN104292122B (en) | In the production of acetoacetanilide, reduce by product 3-(phenyl amino)-2-butylene acetoacetic ester generate method | |
| CN101092352A (en) | Method for refining o - benzoylbenzoic acid | |
| CN107573264A (en) | A kind of preparation technology of the sulfonic acid chloride of 3 cyano group, 5 methoxybenzene 1 | |
| CN102212343A (en) | Preparation method of lithium bromide absorption cycle working fluid | |
| CN112300102B (en) | Synthetic method of furan ammonium salt | |
| CN109678853B (en) | Preparation process of dasatinib | |
| CN104496825B (en) | The preparation method of 2-fluorine ethylamine hydrochloride | |
| CN104619681A (en) | Method for producing (r)-1,1,3-trimethyl-4-aminoindane | |
| CN104119247B (en) | A kind of preparation method of 4 chlorine, 2,5 dimethoxy AAA | |
| CN103497142A (en) | Preparation method of disperse blue 60 and/or homolog thereof | |
| CN107383418B (en) | A kind of uvioresistant plastic additive and preparation method thereof | |
| CN102936213B (en) | Clean preparation method of 1, 8-dinitro-3, 6-naphthalenedisulfonic acid | |
| CN110590652B (en) | Synthesis method of 2-amino-5-iodopyridine | |
| CN103992285B (en) | The production method of 1-H benzotriazole derivative | |
| CN105439837A (en) | Synthetic method of 6-Bromoisovanillin | |
| CN105859559A (en) | Production method of 3-ethoxy-4-nitrophenol | |
| CN106187864A (en) | A kind of method being prepared high-purity bupivacaine alkali by bupivacaine hydrochloride | |
| CN113004366A (en) | Novel method for producing diammonium glycyrrhizinate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |