Preparation method of high-purity D-glucosamine sulfate

A technology of glucosamine sulfate and glucosamine hydrochloride, which is applied in the field of preparation of high-purity D-glucosamine sulfate, can solve problems such as contraindications for use in patients with hyperkalemia of nephropathy, and achieves less pollution, simple equipment and operation technology. advanced effects

Inactive Publication Date: 2010-09-15
王松叶
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The D-glucosamine sulfate products prepared in the prior art are basically double salt products containing more potassium or sodium, which have certai...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1. A preparation method of high-purity D-glucosamine sulfate, the steps are as follows:

[0025] (1) Dissolving: take alkaline substance and dissolve it in an organic solvent under the protection of one or more protective gases in nitrogen, carbon dioxide, and inert gas to make an alkaline solution, and the dissolution temperature is -5°C; The alkaline solution is: hydride HX or alcoholate RCH of lithium, sodium, potassium, magnesium or calcium metal ions 2 OX solution, wherein: X is lithium, sodium, potassium, magnesium or calcium metal ion, R is hydrogen or C 1 -C 8 ; The molar concentration of alkaline substance in alkaline solution is 2%;

[0026] (2) Free: under the protection of the protective gas described in step (1), D-glucosamine hydrochloride with a purity of not less than 95% is added to the alkaline solution under stirring, and the reaction is made to contain chloride crystals and Mixture of free D-glucosamine;

[0027] (3) Desalination: filter...

Embodiment 2

[0030] Example 2. A preparation method of high-purity D-glucosamine sulfate, the steps are as follows:

[0031] (1) Dissolving: take alkaline substance and dissolve it in organic solvent under the protection of one or more protective gases in nitrogen, carbon dioxide and inert gas to make alkaline solution, and the dissolution temperature is 20°C; Alkaline solution: hydride HX or alcoholate RCH of lithium, sodium, potassium, magnesium or calcium metal ions 2 OX solution, wherein: X is lithium, sodium, potassium, magnesium or calcium metal ion, R is hydrogen or C 1 -C 8 ; The molar concentration of alkaline substance in alkaline solution is 45%;

[0032] (2) Free: under the protection of the protective gas described in step (1), D-glucosamine hydrochloride with a purity of not less than 95% is added to the alkaline solution under stirring, and the reaction is made to contain chloride crystals and Mixture of free D-glucosamine;

[0033] (3) Desalination: filter the mixed so...

Embodiment 3

[0036] Example 3. A preparation method of high-purity D-glucosamine sulfate, the steps are as follows:

[0037] (1) Dissolving: take alkaline substance and dissolve it in organic solvent under the protection of one or more protective gases in nitrogen, carbon dioxide and inert gas to make alkaline solution, and the dissolution temperature is 5° C.; Alkaline solution: hydride HX or alcoholate RCH of lithium, sodium, potassium, magnesium or calcium metal ions 2 OX solution, wherein: X is lithium, sodium, potassium, magnesium or calcium metal ion, R is hydrogen or C 1 -C 8 ; The molar concentration of alkaline substances in the alkaline solution is 10%;

[0038] (2) Free: under the protection of the protective gas described in step (1), D-glucosamine hydrochloride with a purity of not less than 95% is added to the alkaline solution under stirring, and the reaction is made to contain chloride crystals and Mixture of free D-glucosamine;

[0039] (3) Desalination: filter the mi...

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PUM

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Abstract

The invention relates to a preparation method of high-purity D-glucosamine sulfate, which is characterized by comprising the steps of: dissolving: weighting an alkali material into an organic solvent to prepare an alkali solution; freeing: adding the D-glucosamine sulfate with purity not less than 95 percent into the alkali solution under stirring, reacting to prepare a mixed solution containing chloride crystals and free D-glucosamine; desalting: filtering the mixed solution to remove chloride to obtain an organic solution containing the free D-glucosamine; salifying: dropping sulfuric acid into the organic solution obtaining the free D-glucosamine for reacting to prepare the D-glucosamine sulfate; and refining to obtain the finished product. The method has advanced operating process, simple equipment and less pollution; the used organic solvents can be recycled; and the prepared high-purity D-glucosamine sulfate contain no potassium, sodium or chloride ions, has no use contraindication, and is safe to use.

Description

technical field [0001] The invention relates to a preparation method of glucosamine, in particular to a preparation method of high-purity D-glucosamine sulfate. Background technique [0002] According to reports, arthritis has become the number one disabling disease in the world. With the aggravation of arthritis pain and activity restriction, it will lead to temporary or permanent loss of working ability, which will bring great losses to society and economy. D-glucosamine sulfate is highly active and easily absorbed, and is the main matrix of articular cartilage and joint fluid. [0003] There are mainly two types of glucosamine in the prior art, one is D-glucosamine hydrochloride, and the other is D-glucosamine sulfate. Among them, D-glucosamine sulfate is divided into: D-glucosamine sulfate potassium sodium salt and D-glucosamine sulfate. In terms of the treatment effect of arthritis, D-glucosamine hydrochloride has a general effect, and at the same time has relatively ...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00
Inventor 陈延静詹金明王松叶洪义霞
Owner 王松叶
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