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A kind of synthesis method of γ-pga-bn with controllable degree of esterification

A synthesis method and technology of esterification degree, applied in the synthesis field of γ-PGA-Bn, can solve the problems of uncontrollable degree of esterification, waste of organic solvent, long reaction time, etc., to save reaction time, save resources, and facilitate follow-up processing easy effect

Active Publication Date: 2022-03-01
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a synthetic method of γ-PGA-Bn with a controllable degree of esterification, which solves the problems of poor solubility, long reaction time, uncontrollable degree of esterification and excessive The problem of wasting organic solvents

Method used

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  • A kind of synthesis method of γ-pga-bn with controllable degree of esterification
  • A kind of synthesis method of γ-pga-bn with controllable degree of esterification

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Embodiment 1

[0022] A method of synthesizing γ-PGA-BN of esterification degree, including the following steps:

[0023] (1) γ-polyglycine raw material (molecular weight is above 700,000) Purification: Take γ-PGA in water, adjusting the pH of 1 by HCl, and then placed in dialysis bag 4 days after dialysis 4 days after lyophilization;

[0024] (2) Synthesis of γ-PGA-BN: Take step (1) Purification of γ-polyglymunine 0.43 ~ 1g in a 50 ml of Slack, add 10 ~ 20ml to ion, add K 2 CO 3 The solution, then placed in an oil bath at 60 ° C, stirred for 0.5 h, adding brominated, reactive 3 to 12 h to be reacted in the upper layer, and the lower layer has a large amount of white solids, the reaction reaches the end point, close the oil bath, cooling To room temperature, where γ-polyglutamic acid, K 2 CO 3 The mass ratio of the solution and bromide solution is 1: 0.53 ~ 5.35: 1.74 ~ 7.96;

[0025] (3) Wash: The solution obtained by step (2) was washed in an HCl aqueous solution of 0 ° C, pH = 1, and the soli...

Embodiment 2

[0027] A method of synthesizing the γ-PGA-BN of esterification degree, including the steps of: (1) γ-polyglymine raw material (more than 700,000 molecular weight): Polyglatine structural formula as shown in :

[0028]

[0029] The γ-PGA40G was dissolved in water, and pH = 1 was adjusted with HCl. After 4 days of dialysis in the dialysis bag, 20.5 g of solid spare was obtained;

[0030] (2) Synthesis of γ-PGA-BN of esterification degree of esterification:

[0031] Weigh 0.43 g of lyophilized γ-PGA in 25ml Slack, add 10ml to ion water, add 0.23 GK 2 CO 3 The above solution was placed in an oil bath at 60 ° C, stirred for 0.5 h, adding 0.75 g of Brominated benz, reaction for about 3 h, and the upper layer is clarified, and there is a large number of white solids in the lower layer, the reaction reaches the end point, close the oil bath, Cool to room temperature.

[0032] The above solution was washed in an HCl aqueous HCl solution of 0 ° C, 100 mL, pH = 1, and the solid was washed ...

Embodiment 3

[0034] Synthesis of γ-PGA-BN of esterification of 28%:

[0035] Weigh 1 g γ-PGA in the 50ml Slack bottle, add 20ml to ion water, add 0.8 GK 2 CO 3 The above solution was placed in an oil bath at 60 ° C, stirred for 0.5 h, and 1.32 g of Brominated benzyl, the reaction time was about 4 h, and the upper layer was clarified in the upper layer, and the lower layer had a large number of white solids, and the reaction reached the end point, close the oil bath, Cool to room temperature.

[0036] The above solution was washed in an HCl aqueous HCl solution of 0 ° C, 200 mL, pH = 1, and the solid was washed 3 times in deionized water, and finally placed in the Sodet extractor, extract 48h with diethyl ether, dried and vacuum Dry, weighed 1.15 g, yield 96%, and migmetric, esterification degree of 28%.

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Abstract

The invention belongs to the technical field of synthesis of biomedical materials, and specifically discloses a method for synthesizing γ-PGA-Bn with a controllable degree of esterification. The γ-PGA has better solubility in water and is dissolved in water to form an aqueous solution. By joining K 2 CO 3 The amount of benzyl bromide is used to control the pH of the solution to control the end point of the reaction; the amount of benzyl bromide is changed to jointly control the degree of esterification of the reaction. Finally, the solution at the end of the reaction is precipitated in an aqueous HCl solution with pH=1 at 0°C, so that the preparation of γ‑PGA‑Bn is more environmentally friendly, economical and efficient.

Description

Technical field [0001] The invention belongs to the field of biomedical material synthesis, and more particularly to a synthesis method of γ-PGA-BN of esterification degree. Background technique [0002] Glutamic acid is one of the 20 amino acids in the human body, and it is important in the metabolism in the biological body. The gamma-polyglymine (γ-PGA) is a polymer polymer having a peptide bond by a glutamic acid unit through an alpha-amino group and a γ-carboxyl group. γ-polyglycine is also known as natto, polyglycine, better solubility in water, non-toxic, and enzymatic degradation. At present, gamma-polyglycine is large in laboratory synthesis, and can only synthesize a polymer having a small molecular weight, a polymer tens of thousands of tens of thousands of polymers typically produce a variety of Bacillus in bacterial extortion, and their molecular weight is up to There are hundreds of thousands of even millions, with the continuous ingestion of biocompatibility and bio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/48
CPCC08G69/48
Inventor 胡志国黄红潘张怡晨刘迎春王亚鹏李梦珂
Owner HENAN NORMAL UNIV
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