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Refining method for Glycyl-L-tyrosine

A technology of glycoside dipeptide and refining method, which is applied in the chemical industry and can solve the problems of difficult drug injection preparation and many impurities related to glycoside dipeptide.

Inactive Publication Date: 2009-05-13
北京博时安泰科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Glycos dipeptide prepared by the above synthetic method has many impurities and a single impurity is greater than 0.5%, it is difficult to be directly used in the preparation of drug injections, so it is meaningful to invent a simple and easy method for refining glycosipeptide and can create good economic value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The WA-30 resin column is pre-installed, and washed with deionized water until neutral; 14kg of crude glycoside dipeptide is dissolved in 210L of pure water, heated to 65°C and stirred to dissolve, cooled, and then passed through the resin column, and the time for passing the column is controlled at 2 hours, sampling analysis, HPLC area normalization method to calculate the content of the main peak area in the fraction is greater than 99.0%, rinse with 70L of pure water, distill the distillate at 75°C, evaporate the water to dryness under reduced pressure, add 70L of water, dissolve Stir at room temperature and slowly precipitate a large amount of solids, add 140L of ethanol to stir, filter with suction, wash the filter cake with ethanol, and dry under reduced pressure at 65°C for 12 hours to obtain the refined product of ganase dipeptide, the purity of ganase dipeptide is 99.8%.

Embodiment 2

[0018] The WA-30 resin column is pre-installed, and washed with deionized water until neutral; 10kg of crude glycoside dipeptide is dissolved in 150L of pure water, heated to 60°C and stirred to dissolve, cooled, and then passed through the resin column, and the time for passing the column is controlled at 1 hour, sampling analysis, HPLC area normalization method to calculate the main peak area content in the fraction is greater than 99.0%, rinse with 50L of pure water, distill the distillate at 70°C, evaporate the water to dryness under reduced pressure, add 50L of water, dissolve Stir at room temperature and slowly precipitate a large amount of solids, add 100L ethanol to stir, filter with suction, wash the filter cake with ethanol, and dry under reduced pressure at 60°C for 10 hours to obtain the refined product of ganase dipeptide. The purity of ganase dipeptide is 99.1%.

Embodiment 3

[0020] D301 resin column is pre-installed, and washed with deionized water until neutral; 6kg of crude glycoside dipeptide is dissolved in 90L of pure water, heated to 70°C and stirred to dissolve, cooled, and then passed through the resin column, and the time for passing the column is controlled at 1.5 hours , sampling analysis, HPLC area normalization method to calculate the main peak area content in the fraction is greater than 99.0%, rinse with 30L pure water, distillate at 80 ° C, evaporate the water to dryness under reduced pressure, add 30L water, dissolve, room temperature Stir and slowly precipitate a large amount of solids, add 60L of ethanol to stir, filter with suction, wash the filter cake with ethanol, and dry under reduced pressure at 65±5°C for 12±2 hours to obtain the refined ganase dipeptide, the purity of which is 99.3%.

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PUM

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Abstract

The invention discloses a method for purifying glycyl-L-tyrosine. Researchers find through experimental researches that the glycyl-L-tyrosine is purified by WA-30 resin column with time flowing column in 2 hours, so that purity of the obtained glycyl-L-tyrosine is more than 99 percent, and single impurity is not more than 0.5 percent. The purification process not only has the advantages of higher yield and lower cost, but also has easily controlled purification process, and is easy for industrialized production.

Description

Technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for refining glycoside dipeptide. Background technique [0002] The Chinese name of glycyl-L-tyrosine is glycyl-L-tyrosine. At present, the method of preparing glycyl-L-tyrosine mostly uses L-tyrosine ester and N-protected glycine as the starting point. The raw materials are condensed into peptides, but the condensing agent used and the method of deprotection are different. According to the literature retrieved, the production is more feasible, which can be roughly summarized as the following three routes: Route 1 Reference Paul, R. et al., Journal Organic Chemistry Vol27: 2094-99 (1962), with N, N'-carbon Acyldiimidazole is used as a condensing agent to condense benzyloxycarbonylglycine and tyrosine ethyl ester to form a peptide, and then hydrolyze the protecting group to obtain glycyl-L-tyrosine. Route 2 References S.Rajappa, K et al., Tetrahedr...

Claims

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Application Information

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IPC IPC(8): C07K1/20
Inventor 颜文革漆新国张典鹏阚迎昕
Owner 北京博时安泰科技发展有限公司