Preparation method of glycyl-tyrosine

A technology of tyrosine and glycyl, which is applied in the field of preparation of glycyl-tyrosine, can solve the problem of high difficulty in the preparation method of glycyl-tyrosine, low yield of glycyl tyrosine crude product, and inconvenience. Industrialization and other problems, to achieve the effect of high solvent recovery rate, cheap raw materials and simple equipment requirements

Inactive Publication Date: 2012-10-10
JIANGSU CHENGXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of glycyl-tyrosine is very difficult. Patent 200810239035.5 discloses a refining method of glycoside dipeptide. In the crude glycoside dipeptide production process, concentrated ammonia, water, ammonium bicarbonate, N- Chloroacetyl-L-tyrosine produces crude glycoside dipeptide under certain conditions. The yield of crude glycoside dipeptide prepared by this process is low, the cost is high, and it is not easy to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 24g of L-tyrosine, 52g of toluene, and 24g of water, put them in a glass bottle and stir evenly, place an ice-water bath outside, and control the temperature at 0°C; add sodium hydroxide solution dropwise, the temperature of the dropping process is controlled at 0°C, and the dropwise addition is completed Finally, stir and react for 30 minutes; add 24 g of chloroacetyl chloride dropwise, and at the same time add dropwise sodium hydroxide solution, the temperature is controlled at -5 ° C, and the pH of the solution is controlled at 11; after the dropwise addition, stir for 30 minutes, and then stand for 1 hour; After standing still, take the lower aqueous phase and pour it into a conical flask, slowly add hydrochloric acid dropwise to control the pH of the solution to 2.5; wait for the crystals to precipitate, and after standing for 1 hour to grow the crystals, centrifuge to obtain the chloroacetyl-tyrosine solid. Take 38.5 g of the obtained chloroacetyl-tyrosine sol...

Embodiment 2

[0019] Take 240g of L-tyrosine, 520g of toluene, and 240g of water, put them in a glass bottle and stir evenly, put an ice-water bath outside, and control the temperature at 5°C; add sodium hydroxide solution dropwise, the temperature of the dropping process is controlled at 5°C, and the dropwise addition is completed Afterwards, stir and react for 35 minutes; add dropwise 240 g of chloroacetyl chloride, and dropwise add sodium hydroxide solution at the same time, the temperature is controlled at 5 ° C, and the pH of the solution is controlled at 13; after the dropwise addition, stir for 50 minutes, and then stand for 1.5 hours; After placing, take the lower aqueous phase and pour it into a conical flask, slowly add hydrochloric acid dropwise, and control the pH of the solution to 3.0; wait for crystals to precipitate, and after standing for crystal growth for 2 hours, centrifuge to obtain chloroacetyl-tyrosine solid, take Put 400g of the obtained chloroacetyl-tyrosine solid in...

Embodiment 3

[0021] Take 500g of L-tyrosine, 1000g of toluene, and 500g of water, put them in a glass bottle and stir evenly, put an ice-water bath outside, and control the temperature at 2°C; add sodium hydroxide solution dropwise, the temperature of the dropping process is controlled at 3°C, and the dropwise addition is completed Finally, stir and react for 40 minutes; add 500 g of chloroacetyl chloride dropwise, and at the same time add dropwise sodium hydroxide solution, the temperature is controlled at 0 ° C, and the pH of the solution is controlled at 12; After placing, take the lower aqueous phase and pour it into a conical flask, slowly add hydrochloric acid dropwise to control the pH of the solution to 3.5; wait for the crystals to precipitate, and after standing for crystal growth for 2 hours, centrifuge to obtain the chloroacetyl-tyrosine solid, take Put 800g of the obtained chloroacetyl-tyrosine solid into a light bulb bottle, add 450g of ammonium bicarbonate and water, and stir...

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PUM

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Abstract

The invention relates to a preparation method of glycyl-tyrosine, which comprises the following steps: using L-tyrosine, toluene and water raw material, adding chloroacetamide and sodium hydroxide drop by drop under certain condition, adding hydrochloric acid drop by drop to control the pH value after reacting, then carrying out an aminolysis at normal pressure, heating and concentrating, washing and centrifuging to obtain the glycyl-tyrosine crude product, dissolving, filtering, crystallizing, carrying out pumping filtration and drying to obtain glycyl-tyrosine. The glycyl-tyrosine crystal prepared by the preparation method has high purity, and is beneficial to further purifying and refining glycyl-tyrosine.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a preparation method of glycyl-tyrosine. Background technique [0002] The clinically used compound amino acid (15) dipeptide (2) injection is a parenteral nutrition preparation, which provides amino acids through parenteral nutrition. It is applied to patients who cannot take oral or enteral nutrition, and whose nutrition cannot meet their needs, especially those with high catabolism. The amino acid exists in the form of dipeptides of glycyl-glutamine and glycyl-tyrosine (Glycyl-L-Tyrosine Dihydratc, referred to as glycyl-tyrosine dipeptide). Two dipeptides (glycyl-glutamine, glycyl-tyrosine) are used to provide glutamine and tyrosine to facilitate protein synthesis. The two polypeptides are directly and completely decomposed into three free amino acids, glycine, glutamine and tyrosine in the body. The compound amino acid (15) dipeptide (2) injection promotes protei...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/062
Inventor 邢将军华俊国周红航
Owner JIANGSU CHENGXIN PHARMA
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