A kind of preparation method of aspartic acid ornithine

A technology of ornithine aspartate and ornithine aspartate is applied in the field of preparation of ornithine aspartate, and can solve the problems of not very huge difference in properties, low purity, difficult recycling of waste liquid, and the like, To achieve the effect of relatively low solvent toxicity, simple post-processing process, and reduction of human injury

Inactive Publication Date: 2017-03-08
北京众和民健医药科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses highly toxic barium ions, and the barium ion removal process is cumbersome
[0008] 4. Chinese patent CN101798275A uses L-ornithine acetate to directly add L-aspartic acid, and then adds ammonia to utilize ammonium acetate and aspartic acid The dissolution of ornithine salt in the solvent is different for refining. This method requires a large amount of solvent, and the properties of the two salts are not very different. The effect of removing ammonium acetate is not very good.
[0010]6. Chinese patent CN102964261 uses ornithine hydrochloride and sodium hydroxide to adjust the pH, and then removes sodium chloride by electrodialysis. This method generates chlorine gas at the anode. Chlorine is very active, and it is very easy to react with ornithine, especially the amino group in ornithine, and the generated by-products no longer move to the electrode and flow out with ornithine, and its properties are similar to those of ornithine. Amino acids are very close, making refining difficult
[0011] 7. Using ornithine hydrochloride as raw material, use ion exchange resin to remove chloride ions, then elute with ammonia water, then heat to remove ammonia, and then add aspartic acid to form a salt. This method is time-consuming, expensive and requires a large amount of Acid-base, large pollution, and when heating to remove ammonia, L-ornithine is unstable under alkaline conditions and easily produces impurities
[0012] From the above prior art, it can be seen that the current method for preparing ornithine-aspartate or solvent consumption is large, the operation is cumbersome, and the purity is not high. It needs post-processing steps such as decolorization and purification, and the subsequent waste liquid is difficult to directly recycle, which affects its industrialized production

Method used

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  • A kind of preparation method of aspartic acid ornithine

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Effect test

Embodiment 1

[0037] Add ornithine hydrochloride (168.62g, 1mol) and aspartic acid (133.10g, 1mol) into the reaction kettle, add 603ml of water, raise the temperature to 30°C, start vacuuming with a water vacuum pump, and keep the pressure below 4000Pa During this period, water is continuously added to keep the liquid level of the reaction liquid near the initial position. As the vacuuming progresses, the internal pressure continues to decrease. After 1 hour of vacuuming, the internal pressure reaches about 3400Pa. Use a nitrate test solution to detect the content of chlorine ions in the extracted gas dissolved in water every 30 minutes. When the extracted gas has no chlorine , the reaction ends.

[0038] The reaction solution was added dropwise to 4.5L of methanol, and a large amount of precipitate was formed. After the dropwise addition was completed, it was stirred for 30 minutes, and filtered with suction to obtain the crude product of aspartic acid ornithine (260g), with a yield of abo...

Embodiment 2

[0041] Add ornithine hydrochloride (168.62g, 1mol) and aspartic acid (133.10g, 1mol) into the reaction kettle, add 900ml of ethanol, heat up to 50°C, start vacuuming with a water vacuum pump, and keep the pressure below 2000Pa During this period, ethanol was continuously added to keep the liquid level of the reaction solution near the initial position. As the vacuuming progresses, the internal pressure continues to decrease. After 1 hour of vacuuming, the internal pressure reaches about 1400Pa. Use a nitrate test solution to detect the content of chlorine ions in the extracted gas dissolved in water every 30 minutes. When the extracted gas has no chlorine , the reaction ends.

[0042] After the reaction, a large amount of precipitates were formed in the reaction solution, and the crude product of ornithine aspartate (258 g) was obtained by suction filtration, with a yield of about 97.2%.

[0043] Dissolve 258g of ornithine aspartic acid crude product in 500ml of water, add it d...

Embodiment 3

[0045] Add ornithine hydrochloride (168.62g, 1mol) and aspartic acid (133.10g, 1mol) into the reaction kettle, add 700ml of water, raise the temperature to 80°C, start vacuuming with a water vacuum pump, and keep the pressure below 500Pa During this period, water is continuously added to keep the liquid level of the reaction liquid near the initial position. As the vacuuming progresses, the internal pressure continues to drop. After 1 hour of vacuuming, the internal pressure reaches about 10Pa. Use a nitrate test solution to detect the content of chlorine ions in the extracted gas dissolved in water every 30 minutes. When the extracted gas has no chlorine , the reaction ends.

[0046] The reaction solution was added dropwise to 4.5L ethanol, a large amount of precipitate was formed, after the dropwise addition was completed, it was stirred for 30 minutes, and filtered with suction to obtain the crude product of aspartic acid ornithine (260g), with a yield of about 98%.

[004...

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Abstract

The invention discloses a method for preparing ornithine aspartate, wherein the method comprises the steps: ornithine hydrochloride and aspartic acid undergo a reaction in the presence of a polar solvent to prepare ornithine aspartate, hydrochloric acid gas is continuously pumped out during the reaction process, and at the same time, the polar solvent is continuously added into the reaction system to maintain the polar solvent volume close to or equal to the initial added volume. The method is simple in steps and easy to operate; the two raw materials are directly added to prepare the product at one step, reaction by-products are few, the post-treatment process is simple, the later purification difficulty is simplified, the obtained ornithine aspartate yield is high, the purity is high, the problems in the prior art of tedious ornithine aspartate preparation, high cost and complicated dealing are overcome, and the difficulty for preparing ornithine aspartate is greatly reduced; and the reaction has no need of large amounts of solvent, the solvent has low relative toxicity, the harm to human bodies is reduced, and the cost of production is also reduced.

Description

technical field [0001] The invention relates to a preparation method of ornithine-aspartate for treating liver diseases, belonging to the technical field of medicine preparation. Background technique [0002] Aspartic Acid Ornithine, the chemical name is Aspartic Acid Ornithine, which is prepared by the German Maxwell Pharmaceuticals. It was first launched in the United States in July 2009. It can protect the stability of the liver cell membrane and improve the microcirculation of the liver tissue. , is beneficial to the energy supply of liver cells, clears capillary ducts, promotes bile excretion, promotes liver cell regeneration, restores liver cell functions, protects and promotes the recovery of mitochondria and rough endoplasmic reticulum, and has the ability to enhance Kupffer cells Function and the protective effect on the liver cell membrane, can improve the stasis of gallbladder, shorten the course of the disease, and increase the cure rate. It is mainly used clinic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/26C07C229/24C07C227/18
Inventor 不公告发明人
Owner 北京众和民健医药科技有限公司
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