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Preparation method of D-glucosamine sulfate sodium chloride salt

A technology of glucosamine hydrochloride and glucosamine, which is applied in the field of preparation of D-glucosamine sulfate sodium chloride salt, can solve problems such as product non-conformity, easy decomposition, and product quality decline, and achieves a novel and unique method and simple process Reasonable and good product quality

Active Publication Date: 2013-01-02
JIANGSU AOXIN BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And this kind of complex is not a stable compound, it is easy to decompose under the condition of heat, the quality of the product is reduced, and the product does not meet the USP Pharmacopoeia standard
Moreover, a large amount of toxic and harmful organic solvents are used in the whole process, resulting in these toxic and harmful residues in the product, which affect the physical and mental health of the human body.

Method used

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  • Preparation method of D-glucosamine sulfate sodium chloride salt
  • Preparation method of D-glucosamine sulfate sodium chloride salt
  • Preparation method of D-glucosamine sulfate sodium chloride salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1, a kind of preparation method of D-glucosamine sulfate sodium chloride salt, its steps are as follows:

[0027] (1) Dissolving: Dissolve D-glucosamine hydrochloride in a solvent; the solvent is selected from water, methanol, ethanol, propanol, isopropanol, n-butanol, tert-butanol, tert-amyl alcohol, acetone , tetrahydrofuran, dioxane, dimethylsulfoxide, N,N-dimethylformamide;

[0028] (2) Free: Add the solution obtained in step (1) at -40°C with sodium-containing alkaline substances or add it under the protection of one or more protective gases in nitrogen, carbon dioxide, and inert gases, and keep it at -40°C ℃, add sodium-containing alkaline substances; the sodium-containing alkaline substances are selected from sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium hydride, sodium methoxide, sodium ethoxide, sodium propoxide, sodium n-butoxide, tert-butyl Sodium alkoxide, sodium tert-amylate;

[0029] (3) Salt formation and complexation...

Embodiment 2

[0032] Embodiment 2, a kind of preparation method of D-glucosamine sulfate sodium chloride salt, its steps are as follows:

[0033] (1) Dissolving: Dissolve D-glucosamine hydrochloride in a solvent; the solvent is selected from water, methanol, ethanol, propanol, isopropanol, n-butanol, tert-butanol, tert-amyl alcohol, acetone , tetrahydrofuran, dioxane, dimethylsulfoxide, N,N-dimethylformamide;

[0034] (2) Freeing: add the solution obtained in step (1) at 100°C with sodium-containing alkaline substances or under the protection of one or more protective gases in nitrogen, carbon dioxide, and inert gases, and keep at 90°C. Add sodium-containing alkaline substances; the sodium-containing alkaline substances are selected from sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium hydride, sodium methoxide, sodium ethoxide, sodium propoxide, sodium n-butoxide, sodium tert-butoxide , sodium tert-amylate;

[0035] (3) Salt formation and complexation: keep the solu...

Embodiment 3

[0038]Example 3, the method of drying or crystallizing the filtrate described in step (4) of the preparation method described in Example 1 or 2 is selected from the following methods: vacuum freeze-drying; spray drying; adding one or more undesirable The solvent is crystallized, filtered, and then dried; after concentration, one or more poor solvents are added for crystallization, filtered, and then dried; the poor solvent is selected from dichloromethane, chloroform, methanol, ethanol, propanol, isopropyl Alcohol, n-butanol, tert-butanol, tert-amyl alcohol, acetone, tetrahydrofuran, dioxane, dimethylsulfoxide, acetonitrile, N,N-dimethylformamide.

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Abstract

The invention discloses a preparation method of D-glucosamine sulfate sodium chloride salt. The preparation method comprises the following steps of: dissolving D-glucosamine hydrochloride in a solvent; adding a sodium-containing alkaline substance into the obtained solution at the temperature of minus 40-100 DEG C, or adding the sodium-containing alkaline substance into the obtained solution under the protection of one or more protective gas(s) of nitrogen, carbon dioxide and inert gases; adding the sodium-containing alkaline substance into the mixed solution at the maintained temperature of minus 40-90 DEG C; adding sulfuric acid into the obtained solution at the temperature of minus 25 to 90 DEG C for salifying; carrying out complexation reaction to obtain a D-glucosamine sulfate sodium chloride salt complex; and filtering and crystallizing to obtain the D-glucosamine sulfate sodium chloride salt solid. The method is novel and unique and simple and reasonable in technology, product quality is good and purity is high, and completely reaches the standard of United States patent (USP) 34 edition pharmacopeia.

Description

technical field [0001] The invention relates to a preparation method of sodium salt, in particular to a preparation method of D-glucosamine sulfate sodium chloride salt. Background technique [0002] D-glucosamine sulfate sodium chloride salt was first recorded in the 27th edition of the United States Pharmacopoeia, and it is a drug for treating arthritis. Arthritis has become the number one disabling disease in the world, with exacerbated arthritis pain and impaired mobility leading to temporary or permanent incapacity to work. Bringing great losses to the society and economy, D-glucosamine sulfate sodium chloride salt is more and more widely used in the treatment of arthritis because of its high activity and easy absorption. It is the main matrix of articular cartilage and joint fluid. [0003] There are mainly two types of D-glucosamine in the prior art, one is D-glucosamine hydrochloride, and the other is D-glucosamine sulfate. In terms of the treatment effect of arthr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06C07H1/00
Inventor 陈延静詹金明王松叶欧瑞
Owner JIANGSU AOXIN BIOTECHNOLOGY CO LTD
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