CN103880663A - Aspirin preparation method - Google Patents
Aspirin preparation method Download PDFInfo
- Publication number
- CN103880663A CN103880663A CN201210565499.1A CN201210565499A CN103880663A CN 103880663 A CN103880663 A CN 103880663A CN 201210565499 A CN201210565499 A CN 201210565499A CN 103880663 A CN103880663 A CN 103880663A
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- CN
- China
- Prior art keywords
- solid
- aspirin
- diacetyl oxide
- acetylsalicylic acid
- ion liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an aspirin preparation method. The method comprises the following steps: mixing salicylic acid with a catalyst and acetic anhydride, heating, carrying out constant temperature stirring at 65-85DEG C for 25-55min, adding ice water for dissolving acetic anhydride, cooling acetic anhydride in an ice water bath for 25min to precipitate a solid, carrying out pumping filtration, washing with cold water, and dewatering to obtain crude aspirin; adding a saturated sodium carbonate solution, stirring until no bubbles exist, and filtering to remove insoluble substances; dumping the obtained filtrate into a beaker containing concentrated sulfuric acid, and stirring to gradually precipitate a solid; cooling the obtained solid in the ice water bath, carrying out pumping filtration after the solid completely precipitates, and drying to obtain an aspirin product. The method has the advantages of realization of no equipment corrosion or latent pollution by using the catalyst, high product yield, and repeatable use of the catalyst.
Description
The present invention relates to a kind of method of preparing acetylsalicylic acid, particularly relate to a kind of method that catalyzes and synthesizes acetylsalicylic acid with ionic liquid replacement concentrated sulfuric acid catalyst.
Background technology
Acetylsalicylic acid (Aspirin, acetylsalicylic acid, formal name used at school: 2-Aspirin) is a kind of conventional bring down a fever anodyne and antirheumatic medicine, acetylsalicylic acid energy effectively preventing arteriosclerosis, anticoagulant.Aspect prevention and cure of cardiovascular disease, there is good effect, can also make the possibility of gallbladdergallstonecholetithiasis reduce 55%, make people suffer from cataractous possibility and reduce 75%, effect that can Breast Cancer Prevention, lung cancer, also has good effect to skin carcinoma.After acetylsalicylic acid is decomposed, can become salicylate, it can stop the formation of free radical, thus deaf generation due to prevention aminoglycosides antibiotics.Meanwhile, its dilute solution is used for watering fruit tree, has the effects such as the fallen flowers of minimizing, shedding, increase fruiting rate.Therefore, the demand of acetylsalicylic acid increases day by day.
The synthetic method of traditional acetylsalicylic acid is to carry out under O-acylation reaction synthetic with Whitfield's ointment and diacetyl oxide in the katalysis of the vitriol oil; but; the vitriol oil has larger corrodibility to equipment; more dangerous in use procedure; spent acid solution is large to environment; and easily there is side reaction and make product color dark, be unfavorable for purifying.Thereby find a class new catalytic activity catalyzer high, environment-friendly type and replace protonic acid to catalyze and synthesize acetylsalicylic acid having become the new problem of people's research.Ionic liquid at room temperature is the novel environmental friendly catalyst that a class of rising in recent years has application prospect, because it has that liquid wide ranges, soluble end are wide, vapour pressure is zero, good stability, acid-basicity is adjustable, product is easily separated and a series of peculiar properties such as reusable edible, is considered to another large class after water and supercritical CO 2 and has in modern organic synthesis novel green solvent, the catalyzer of applications well prospect.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing acetylsalicylic acid, the method utilization does not have the ionic-liquid catalyst green of corrodibility and potentially contaminated, efficiently prepares acetylsalicylic acid.
The object of the invention is to be achieved through the following technical solutions:
A kind of method of preparing acetylsalicylic acid, this preparation method comprises the following steps: Whitfield's ointment, catalyzer and diacetyl oxide three are mixed, after heated constant temperature stirs, stir after 25 ~ 55 minutes 65 ~ 85 ℃ of heated constant temperature, add frozen water, dissolve diacetyl oxide, diacetyl oxide is placed in ice-water bath cooling 15 minutes, separates out solid suction filtration, with cold water washing, drain, obtain the thick product of acetylsalicylic acid;
Add saturated sodium carbonate solution, be stirred to without bubble, elimination insolubles; Filtrate pouring into filled in the beaker of the vitriol oil, and stir, have solid to separate out gradually; Solids is placed in to ice-water bath cooling, suction filtration after solids is separated out completely, dry, obtain aspirin product.
A kind of described method of preparing acetylsalicylic acid, catalyzer described in it is amino acid ion liquid, for the one in glycine hydrogen sulfate ion liquid or L-glutamic acid hydrogen sulfate ion liquid or L-Ala hydrogen sulfate ion liquid, consumption is 15% ~ 35% of Whitfield's ointment quality.
A kind of described method of preparing acetylsalicylic acid, the diacetyl oxide consumption described in it is 1.5 ~ 3.5 times of Whitfield's ointment mole number.
The invention has the advantages that: (1) product yield is high, reaches 85% left and right.
(2) product purity is high, purity >99.9%
(3) catalyzer can not cause the corrosion of equipment and potential pollution.
(4) catalyzer can be reused.
Claims (3)
1. prepare the method for acetylsalicylic acid for one kind, it is characterized in that, this preparation method comprises the following steps: Whitfield's ointment, catalyzer and diacetyl oxide three are mixed, after heated constant temperature stirs, stir after 25 ~ 55 minutes 65 ~ 85 ℃ of heated constant temperature, add frozen water, dissolve diacetyl oxide, diacetyl oxide is placed in ice-water bath cooling 15 minutes, separate out solid suction filtration, with cold water washing, drain, obtain Ah
The thick product of a department woods; Add saturated sodium carbonate solution, be stirred to without bubble, elimination insolubles; Filtrate pouring into filled in the beaker of the vitriol oil, and stir, have solid to separate out gradually; Solids is placed in to ice-water bath cooling, suction filtration after solids is separated out completely, dry, obtain aspirin product.
2. according to a kind of method of preparing acetylsalicylic acid described in claim 1, it is characterized in that, described catalyzer is amino acid ion liquid, for the one in glycine hydrogen sulfate ion liquid or L-glutamic acid hydrogen sulfate ion liquid or L-Ala hydrogen sulfate ion liquid, consumption is 15% ~ 35% of Whitfield's ointment quality.
3. according to a kind of method of preparing acetylsalicylic acid described in claim 1, it is characterized in that, described diacetyl oxide consumption is 2.0 ~ 3.0 times of Whitfield's ointment mole number.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210565499.1A CN103880663A (en) | 2012-12-24 | 2012-12-24 | Aspirin preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210565499.1A CN103880663A (en) | 2012-12-24 | 2012-12-24 | Aspirin preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103880663A true CN103880663A (en) | 2014-06-25 |
Family
ID=50949833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210565499.1A Pending CN103880663A (en) | 2012-12-24 | 2012-12-24 | Aspirin preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103880663A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086418A (en) * | 2014-07-14 | 2014-10-08 | 山东省泰和水处理有限公司 | Method for preparing acetyl salicylic acid |
| CN104829453A (en) * | 2015-05-11 | 2015-08-12 | 江苏天晟药业有限公司 | Preparation method of acetylsalicylic acid |
| CN108727188A (en) * | 2018-07-13 | 2018-11-02 | 黄河水利职业技术学院 | A kind of method of new catalyst synthesis aspirin |
-
2012
- 2012-12-24 CN CN201210565499.1A patent/CN103880663A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086418A (en) * | 2014-07-14 | 2014-10-08 | 山东省泰和水处理有限公司 | Method for preparing acetyl salicylic acid |
| CN104829453A (en) * | 2015-05-11 | 2015-08-12 | 江苏天晟药业有限公司 | Preparation method of acetylsalicylic acid |
| CN108727188A (en) * | 2018-07-13 | 2018-11-02 | 黄河水利职业技术学院 | A kind of method of new catalyst synthesis aspirin |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140625 |