Preparation method of L-carnosine zinc

A technology of carnosine zinc and carnosine, which is applied in the field of preparation of pharmaceutical intermediates, can solve the problems of low utilization rate of raw materials, high residual salt content, large solvent consumption, etc., and achieves the effects of reducing preparation cost, good yield and stable quality

Active Publication Date: 2010-03-03
SUZHOU FUSHILAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, the above-mentioned process has the defects of large solvent consumption, low utilization rate of raw materials, and high residual salt content in the product.

Method used

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  • Preparation method of L-carnosine zinc
  • Preparation method of L-carnosine zinc

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Get 2.5g of L-carnosine with an optical purity of more than 99.5%, dissolve it with 500g of pure water, and get the commodity model D201 macroporous anion-exchange resin prepared in advance, preferably but not limited to, produced by Langfang New Times Chemical Co., Ltd., Hebei Province, China That is, 100 g of macroporous basic anion exchange resin is dropped into the above-mentioned L-carnosine aqueous solution, stirred for 2.0 h (static adsorption), the temperature is controlled at 5-10 ° C, the adsorbed resin is packed into a column, and the mass percentage concentration is 2% ZnCl 2 Reverse elution with aqueous solution, the temperature during elution is controlled at 15-20°C, and the elution rate is controlled at 5.0-6.0vvh -1 . As the elution proceeds, the generated L-carnosine zinc is precipitated from the aqueous solution. When no solid is washed out in the eluent, the eluent containing L-carnosine zinc is combined, and dried at 80°C after solid-liquid separati...

Embodiment 2

[0028] Get the L-carnosine 5.0g more than 99.5% of optical purity, dissolve with 500g pure water, get the ion-exchange resin 100g described in embodiment 1 of pretreatment and drop into above-mentioned L-carnosine aqueous solution, stir 2.0h (static adsorption: Static adsorption The specified amount of adsorbent and quantitative solution reach equilibrium after a long time of full contact.), the temperature is controlled at 5-10 ° C, the adsorbed resin is packed into a column, and ZnCl with a zinc ion mass concentration of 2% 2 Reverse elution with aqueous solution, the temperature during elution is controlled at 20-30°C, and the elution rate is controlled at 5.0-6.0vvh -1 . As the elution proceeds, the generated L-carnosine zinc is precipitated from the aqueous solution. When no solid is washed out in the eluent, the eluent containing L-carnosine zinc is combined, and after solid-liquid separation, it is dried at 80°C to obtain L- Carnosine zinc product 6.2g. Mass yield: 12...

Embodiment 3

[0030] Get L-carnosine 20g more than 99.5% of optical purity, dissolve with 1000g pure water, get pretreated D201 (commercial model, macroporous anion exchange resin is macroporous basic anion exchange resin) ion exchange resin 200g packing column, will The above-mentioned carnosine solution passes through the installed ion-exchange column for adsorption and activation (dynamic adsorption), the temperature is controlled at 0-5°C, and the flow rate is controlled at 1.0vvh -1 , after the activation of the carnosine solution on the column, use ZnCl with a zinc ion mass concentration of 2% 2 Reverse elution with aqueous solution, the temperature during elution is controlled at 20-30°C, and the elution rate is controlled at 5.0-6.0vvh -1 . As the elution proceeds, the generated L-carnosine zinc is precipitated from the aqueous solution. When no solid is washed out in the eluent, the eluent containing L-carnosine zinc is combined, and after solid-liquid separation, it is dried at 8...

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Abstract

The invention relates to a preparation method of L-carnosine zinc, which belongs to the technical field of preparation of pharmaceutical intermediates. The preparation method comprises the steps of dissolving L-carnosine in water for forming water solution of the L-carnosine, leading the water solution of the L-carnosine to be reacted with ion exchange resin for absorbing the L-carnosine on the resin for activation, adopting the water solution of zinc salt for eluting the resin absorbed with the L-carnosine, combining zinc ions in eluent with the activated L-carnosine molecules for forming L-carnosine zinc, precipitating from the water and carrying out solid-liquid separation on the eluent, thereby obtaining the L-carnosine zinc. The preparation method has the advantages that the technicalscheme for preparing the L-carnosine zinc has good yield, the zinc content in a product is not less than 22.0%, the optical rotation is not less than plus 8.0 degrees, and the quality is stable; andthe technical scheme does not use an organic solvent, the used ion exchange resin is recycled, and the main raw material of the L-carnosine is completely reacted, thereby improving the utilization rate of raw materials, reducing the preparation cost and meeting the industrial production requirements.

Description

technical field [0001] The invention belongs to the technical field of preparation of pharmaceutical intermediates, in particular to a method for preparing L-carnosine zinc, more specifically a method for preparing L-carnosine zinc by means of ion exchange. Background technique [0002] The properties of L-carnosine zinc are white powder, insoluble in water, hardly soluble in organic solvents; molecular formula is C 9 h 12 N 4 o 3 Zn; The English chemical name of L-carnosine zinc is: Zinc N-(3-aminopropionyl)histidine, and the structural formula is as follows: [0003] [0004] L-carnosine zinc (L-carnosine zincate), also known as polaprezinc, is a new anti-ulcer drug jointly developed by Japan Hamari Chemical Co., Ltd. and Zeria Pharmaceutical Company. Studies in animal experimental models have shown that L-carnosine zinc can accelerate the healing of chronic gastric ulcers and stimulate the proliferation of epithelial cell layers. Pre-administration of L-carnosine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/64
Inventor 陆建刚邢健严希康腾明清丁建飞陆水元
Owner SUZHOU FUSHILAI PHARMA CO LTD
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