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Preparation method of DL-ornithine DL-aspartate

A technology of aspartic acid and ornithine, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of cyanide reactions, etc., can solve the problems of quantitatively proving the content of chiral isomers, etc., and achieve high yield High, high-purity, easy-to-operate effects

Active Publication Date: 2017-07-25
蚌埠丰原涂山制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the chirality problem in the compound has been controlled by the specific rotation method in the quality standard of L-aspartic acid L-ornithine, the content of chiral isomers cannot be quantitatively proved

Method used

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  • Preparation method of DL-ornithine DL-aspartate
  • Preparation method of DL-ornithine DL-aspartate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the preparation of DL-aspartic acid DL-ornithine

[0025] 1) Add 100 g of L-aspartic acid L-ornithine salt solid to 500 g of acetic acid aqueous solution (50% concentration), stir and dissolve completely, add 10 g of salicylaldehyde to the above solution, heat to 70 ° C and stir for 3.5 h ;

[0026] 2) Heat the solution obtained in step 1) at 50-60°C, add 500g of methanol dropwise, and the dropwise addition time is 2.5h. Crystals are gradually precipitated during the dropwise addition. The solid was dried under vacuum at 45°C for 6 hours to obtain 86.7 g of solid. Yield 86.7%, purity 99.7%.

[0027] Take this product, weigh it accurately, and make a solution containing 80mg per 1ml. The temperature of the test solution should be 20°C±0.5°C, and the specific rotation for detection and calculation should be 0°.

Embodiment 2

[0028] Embodiment 2: the preparation of DL-aspartic acid DL-ornithine

[0029] 1) Add 100 g of L-aspartic acid L-ornithine salt solid into 600 g of acetic acid aqueous solution (40% concentration), stir and dissolve completely, add 8 g of salicylaldehyde to the above solution, heat to 70° C. and stir for 4 h;

[0030] 2) Heat the solution obtained in step 1) at 50°C and add 500g of methanol dropwise. The dropwise addition time is 2h. Crystals are gradually precipitated during the dropwise addition. After drying at ℃ for 6h, 82.4g of solid was obtained. Yield 82.4%, purity 99.6%.

[0031] Take this product, weigh it accurately, and make a solution containing 80mg per 1ml. The temperature of the test solution should be 20°C±0.5°C, and the specific rotation for detection and calculation should be 0°.

Embodiment 3

[0032] Embodiment 3: the preparation of DL-aspartic acid DL-ornithine

[0033] 1) Add 100 g of L-aspartic acid L-ornithine salt solid into 500 g of acetic acid aqueous solution (50% concentration), stir and dissolve completely, add 10 g of salicylaldehyde to the above solution, heat to 65 ° C and stir for 3.5 h ;

[0034] 2) Heat the solution obtained in step 1) at 50-60°C and add 400g of ethanol dropwise for 2.5 hours. During the dropwise addition, crystals are gradually precipitated. After the dropwise addition, keep stirring for 4 hours to grow crystals, cool down to 30°C, and filter to obtain a solid , and vacuum-dried at 45°C for 6h to obtain 84.7g of solid. Yield 84.7%, purity 99.6%.

[0035] Take this product, weigh it accurately, and make a solution containing 80mg per 1ml. The temperature of the test solution should be 20°C±0.5°C, and the specific rotation for detection and calculation should be 0°.

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Abstract

The invention relates to a preparation method of racemate ornithine aspartate. The preparation method comprises the following steps: (1) taking an acetic acid water solution as a solvent, enabling L-ornithine L-aspartate salt to generate racemization reaction under the action of a catalyst to obtain racemization liquid; and (2) adding an anti-solvent into the racemization liquid, crystallizing, filtrating and drying to obtain DL-ornithine DL-aspartate. According to the preparation method provided by the invention, the raw materials are easy to obtain; the operation is simple and convenient, and easy to control; and the preparation process is stable and reliable, so that the preparation method is suitable for mass production of racemate ornithine aspartate samples.

Description

technical field [0001] The invention relates to a preparation method of DL-aspartic acid and DL-ornithine, belonging to the technical field of pharmaceutical engineering. Background technique [0002] DL-Aspartic Acid DL-Ornithine is a chiral impurity that may exist in L-Aspartic Acid L-Ornithine raw materials and preparations. Its structural formula is as follows: [0003] [0004] Although the chirality problem in the compound has been controlled by the method of specific rotation in the quality standard of L-aspartic acid L-ornithine, the content of chiral isomers cannot be quantitatively proved. [0005] In order to accurately detect the content of chiral isomerism in L-aspartic acid L-ornithine raw materials and preparations, so as to ensure the quality of L-aspartic acid L-ornithine, high-purity DL-aspartate is required Amino acid DL-ornithine was used as a working control for detection. Contents of the invention [0006] The purpose of this invention is to pro...

Claims

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Application Information

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IPC IPC(8): C07C227/36C07C227/42C07C229/24C07C229/26
CPCC07C227/36C07C227/42C07C229/24C07C229/26
Inventor 夏继祥张勇刘兆祥单永继张祖杨李保琴胡志国宋强君刘德光
Owner 蚌埠丰原涂山制药有限公司