CN105037185A - Preparation method of potassium aspartate semihydrate - Google Patents
Preparation method of potassium aspartate semihydrate Download PDFInfo
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- CN105037185A CN105037185A CN201510350022.5A CN201510350022A CN105037185A CN 105037185 A CN105037185 A CN 105037185A CN 201510350022 A CN201510350022 A CN 201510350022A CN 105037185 A CN105037185 A CN 105037185A
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- aspartic acid
- semihydrate
- potassium
- preparation
- acid potassium
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Abstract
The invention relates to a method for preparing potassium aspartate semihydrate. In the method, asparaginic acid powder and anhydrous potassium carbonate powder are added into an organic solvent like methanol or acetone and the like according to the molar ratio of 2:1, stirring is performed for reaction, the suction filtration is carried out, and obtained solid powder is dried, so that the potassium aspartate is obtained. Compared with other technologies, the method has the advantages that the process is simple, the energy consumption is relatively low, the production cost is reduced, and the efficiency is improved.
Description
Technical field
The present invention relates to a kind of synthetic method of known compound, relate to a kind of synthetic method of Aspartic acid potassium semihydrate in particular.
Background technology
Potassium L-aspartate has significant curative effect in adjustment myocardial function and the various heart disorder such as electro physiology and treatment cardiovascular and cerebrovascular diseases, hypokalemia, hepatitis, hepatic insufficiency etc., is a kind of medicine intermediate.The semihydrate of what European Pharmacopoeia EP7.0 recorded for medicinal aspartic acid is ASPARTIC ACID monopotassium salt, molecular formula is C
4h
6kNO
41/2H
2o, molecular weight 180.2.The aspartic acid physico-chemical property of this structure is comparatively stable, is applicable to the bulk drug of tablet, injection.
The preparation method of the Aspartic Acid sylvite of current bibliographical information mainly with Aspartic Acid and potassium hydroxide or salt of wormwood for raw material obtains through salify in aqueous phase.
Patent 201210429057.4 reports a kind of preparation method of Aspartic Acid sylvite.The aqueous solution of Aspartic Acid sylvite concentrated removing moisture is obtained Aspartic Acid sylvite supersaturated solution by the method.Then by the aqueous solution of Aspartic Acid sylvite under the high vacuum condition of 4.5 ~ 6.5Pa, obtain in-30 ~-15 DEG C of lyophilizes.
Patent 201210355266.9 reports the preparation method of another kind of different Aspartic Acid sylvite.The method is by certain density Aspartic Acid potassium salt soln, and in control inlet temperature 150 ~ 240 DEG C, under the condition that air outlet temperature is 70 ~ 140 DEG C, spraying dry obtains.
Above-mentioned production technique is that freeze-drying or spray-drying process all exist the high shortcoming of energy consumption, and the product prepared in addition is likely a kind of unformed powder, and water absorbability is comparatively strong, is not suitable for the preparation of tablet.
Summary of the invention
The present invention aims to provide a kind of method preparing Aspartic Acid sylvite, and technical problem to be solved reduces the production energy consumption of Aspartic Acid sylvite, prepares stable C
4h
6kNO
41/2H
2the product of the structure of this crystal formation of O.
Utilize aspartic acid powder and Anhydrous potassium carbonate powder to join in methyl alcohol or acetone and other organic solvent according to mol ratio 2:1, stirring reaction, suction filtration, obtains Aspartic acid potassium by after the drying of gained pressed powder.
Embodiment
Below technical scheme of the present invention is described, so that those skilled in the art understand.
Embodiment one:
In 2L there-necked flask, add methyl alcohol 1.5L, under slowly stirring, add potassium hydroxide 56.1g(1.0moL), Aspartic Acid 133.1g(1.0mol), stirred at ambient temperature 12 hours.Suction filtration, after drying, obtains Aspartic Acid sylvite semihydrate 168.2g, yield 93.3%.
Embodiment two:
In 3L there-necked flask, add methyl alcohol 2.0L, under slowly stirring, add potassium hydroxide 74.8g(1.33moL), Aspartic Acid 177.5g(1.33mol), stirred at ambient temperature 12 hours.Suction filtration, after drying, obtains Aspartic Acid sylvite semihydrate 228.7g, yield 95.2%.
Embodiment three:
In 5L there-necked flask, add methyl alcohol 3.0L, under slowly stirring, add potassium hydroxide 112.2g(2.0moL), Aspartic Acid 266.2g(2.0mol), stirred at ambient temperature 12 hours.Suction filtration, after drying, obtains Aspartic Acid sylvite semihydrate 338.0g, yield 93.8%.
As can be seen from above-mentioned three embodiments, the method for the present patent application is adopted to prepare the yield of aspartic acid all more than 90%, reaction environment and the relatively good control of temperature, lower with other technique phase specific energy consumptions.
Above-mentioned invention to be exemplarily described; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed this insubstantial that method of the present invention is conceived and technical scheme is carried out to improve; or the design of invention and technical scheme directly applied to other occasions, all within protection scope of the present invention without to improve.
Claims (4)
1. the preparation method of an Aspartic acid potassium, with aspartic acid and Anhydrous potassium carbonate for raw material, first Aspartic Acid and salt of wormwood are pulverized respectively, cross 300 mesh sieves, then under the condition separately not adding water, two molecule Aspartic Acids and a part salt of wormwood generation neutralization reaction, and with react a part water of generating and to be directly combined at the organic solvent such as alcohols or ketone and to form Aspartic acid potassium semihydrate.
2. the method preparing Aspartic acid potassium according to claim 1, is characterized in that: described alcoholic solvent is the lower alcohols such as methyl alcohol, ethanol, propyl alcohol, propyl carbinol, and described ketones solvent is the rudimentary ketone such as acetone, butanone.
3. the method preparing Aspartic acid potassium according to claim 1, is characterized in that: the consumption of organic solvent used is about 1 ~ 2 times of Aspartic Acid quality.
4. the method for synthesis Aspartic acid potassium semihydrate according to claim 1, is characterized in that: the mol ratio of aspartic acid and Anhydrous potassium carbonate is 2:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510350022.5A CN105037185A (en) | 2015-06-24 | 2015-06-24 | Preparation method of potassium aspartate semihydrate |
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| CN201510350022.5A CN105037185A (en) | 2015-06-24 | 2015-06-24 | Preparation method of potassium aspartate semihydrate |
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| CN105037185A true CN105037185A (en) | 2015-11-11 |
Family
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117070A (en) * | 2016-06-17 | 2016-11-16 | 宜兴市前成生物有限公司 | A kind of method preparing L asparagine acid disodium |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234992A (en) * | 2008-03-10 | 2008-08-06 | 北京京卫信康医药科技发展有限公司 | Method for preparing aspartic acid |
| CN101239925A (en) * | 2008-03-10 | 2008-08-13 | 北京京卫信康医药科技发展有限公司 | Method for preparing magnesium aspartate |
| CN102408347A (en) * | 2011-10-31 | 2012-04-11 | 宜兴市前成生物有限公司 | Method for preparing monopotassium L-aspartate dihydrate by separation process |
| CN104262185A (en) * | 2014-10-09 | 2015-01-07 | 中国食品发酵工业研究院 | Method for solid-phase synthesis of potassium aspartate at room temperature |
-
2015
- 2015-06-24 CN CN201510350022.5A patent/CN105037185A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234992A (en) * | 2008-03-10 | 2008-08-06 | 北京京卫信康医药科技发展有限公司 | Method for preparing aspartic acid |
| CN101239925A (en) * | 2008-03-10 | 2008-08-13 | 北京京卫信康医药科技发展有限公司 | Method for preparing magnesium aspartate |
| CN102408347A (en) * | 2011-10-31 | 2012-04-11 | 宜兴市前成生物有限公司 | Method for preparing monopotassium L-aspartate dihydrate by separation process |
| CN104262185A (en) * | 2014-10-09 | 2015-01-07 | 中国食品发酵工业研究院 | Method for solid-phase synthesis of potassium aspartate at room temperature |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117070A (en) * | 2016-06-17 | 2016-11-16 | 宜兴市前成生物有限公司 | A kind of method preparing L asparagine acid disodium |
| CN106117070B (en) * | 2016-06-17 | 2018-09-28 | 宜兴市前成生物有限公司 | A method of preparing ASPARTIC ACID disodium |
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Application publication date: 20151111 |