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Preparation method of D-lysine hydrochloride

A technology of lysine hydrochloride and lysine, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc., can solve the problems of no contribution to environmental protection, achieve stable product quality, save concentration Energy consumption, good separation effect

Inactive Publication Date: 2013-07-17
ZHANGJIAGANG HUACHANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007]The two production methods reported so far all adopt ion exchange resin to separate DL-lysine from D-lysine or decompose D-lysine diastereomer body salt and therefore do not contribute to the protection of the environment

Method used

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  • Preparation method of D-lysine hydrochloride
  • Preparation method of D-lysine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method of D-lysine hydrochloride, which comprises the following steps carried out in sequence:

[0044] (1) Take 140mL of DL-lysine solution equivalent to 100g of DL-lysine, add it to a 500mL three-necked flask, heat up to 50℃~60℃ under stirring, then add 75gL-tartaric acid to react to form diastereomers Precipitation of salt L-tartrate D-lysine;

[0045] (2) Filter and separate the precipitate and solution of the diastereomeric salt L-tartrate D-lysine, collect 53.75 g of the diastereomeric salt L-tartrate D-lysine, and set aside;

[0046] (3) Add 25~55g of water to wash the diastereomeric salt L-tartrate D-lysine, filter dry, then add 120g methanol, then wash the diastereomeric L-tartrate D-lysine salt, and then filter Dried to obtain 45g of diastereomer L-tartrate D-lysine salt, set aside;

[0047] (4) Dissolve the diastereomeric salt L-tartrate D-lysine with 1~2 times the mass of water, and then add 13.5g of calcium hydroxide under stirring at room t...

Embodiment 2

[0058] A preparation method of D-lysine hydrochloride, which comprises the following steps carried out in sequence:

[0059] (1) Take 590mL of DL-lysine solution equivalent to 500g of DL-lysine, add it into a 1000mL three-necked flask, heat up to 40°C-50°C under stirring, then add 360gL-tartaric acid to react to form diastereomers Precipitation of salt L-tartrate D-lysine;

[0060] (2) Filter and separate the diastereomeric salt L-tartrate D-lysine precipitate and solution, collect 269.5 g of the diastereomeric salt L-tartrate D-lysine, and set aside;

[0061] (3) Add a proportional amount of water to wash the diastereomer salt L-tartrate D-lysine, filter to dry, then add a proportional amount of methanol, then wash the diastereomer L-tartrate D-lysine salt, and then filter Dried to obtain 226.4g of diastereomer L-tartrate D-lysine salt, set aside;

[0062] (4) Dissolve 226.4g of the diastereomeric salt L-tartrate D-lysine in 2~3 times the mass of water, and then add 78g of ...

Embodiment 3

[0072] A preparation method of D-lysine hydrochloride, which comprises the following steps carried out in sequence:

[0073] (1) Take 1500mL of DL-lysine solution equivalent to 1000g of DL-lysine, add it to a 3000mL three-necked flask, heat up to 30-70°C under stirring, then add 750gL-tartaric acid to react to form diastereomeric salts L-tartrate D-lysine precipitation;

[0074] (2) Filter and separate the precipitate and solution of the diastereomeric salt L-tartrate D-lysine, collect 540 g of the diastereomeric salt L-tartrate D-lysine, and set aside;

[0075] (3) Add 280g of water to wash the diastereomeric salt L-tartrate D-lysine, filter dry, then add 1200g methanol, then wash the diastereomeric L-tartrate D-lysine salt, then filter dry, Obtain 440.7g of diastereomer L-tartrate D-lysine salt, set aside;

[0076] (4) Dissolve 440.7g of the diastereomeric salt L-tartrate D-lysine in 1 to 3 times the mass of water, then add 85g of calcium hydroxide and 70g of calcium carbo...

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Abstract

The invention relates to a preparation method of D-lysine hydrochloride. The method comprises the following steps of: by taking DL-lysine as a raw material, after purification, reacting at 30-70 DEG C with L-tartaric acid to generate diastereomer salt; then, performing inorganic calcium salt with diastereomer salt to generate a calcium tartrate precipitate, while maintaining D-lysine in a liquid; adjusting pH, decoloring, concentrating and crystallizing the D-lysine liquid through hydrochloric acid to obtain D-lysine hydrochloride crude crystalline; and purifying the D-lysine hydrochloride crude crystalline to obtain the D-lysine hydrochloride. The content of DL-lysine in the D-lysine hydrochloride is below 0.5%. According to the method provided by the invention, a simple neutralization precipitation method replaces a complex ion-exchange resin method to the benefit of simplifying the production method and stabilizing the product quality. Meanwhile, the method further has the advantages of no special devices and reduction of environmental pollution, and is easy to popularize and apply industrially.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of D-lysine hydrochloride. Background technique [0002] Lysine and its hydrochloride are an amino acid that is actively developed and continuously expanded at home and abroad. According to the available information, this product is mainly used as a drug intermediate, such as in the synthesis of luteinizing hormone (LH) A precursor of analogs (Proc Natl Acad Sci USA, 1989, 86(16); 6313-6317), a highly active analog of synthetic gonadotropin-releasing hormone (GnRH). Studies have also found that D-lysine can effectively reduce non-enzymatic glycation in the body when used as a clinical drug (Clinical Chemistry, 1989, 35(3); 384-387). The polymer of D-lysine is a good carrier of drugs (J Controlled Release, 1989, 10:89-96). It is also reported that the introduction of 2 to 5 D-lysines in the molecule of antimicrobial peptide CM15 to replace the 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/26C07C227/34
Inventor 王平周锡樑韦平和
Owner ZHANGJIAGANG HUACHANG PHARMA
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