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Method for synthesizing galactose copolymer by adopting RAFT method

A technology of galactose and copolymer, which is applied in the field of preparation of galactose copolymer, can solve the problems of free radical termination reaction and uncontrollable reaction, and achieve the effect of low dispersion width, strong selectivity and high yield

Inactive Publication Date: 2014-09-10
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the traditional free radical polymerization system, the concentration of free radicals is high, and the termination reaction of free radicals is prone to occur, resulting in uncontrollable reactions.

Method used

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  • Method for synthesizing galactose copolymer by adopting RAFT method
  • Method for synthesizing galactose copolymer by adopting RAFT method
  • Method for synthesizing galactose copolymer by adopting RAFT method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Dissolve divinyl adipate and galactose at a molar ratio of 3:1 in 100 mL of anhydrous pyridine, add 0.5 g of alkaline protease, and react in a constant temperature water bath at 50°C and 200 rpm for 4 days to synthesize vinyl Galactosyl adipate (OVNG).

[0029] (2) Dissolve the synthesized OVNG and diethylene glycol dimethacrylate (DEGMA) in 2 mL of DMF, add VAZO-88 as an initiator, and add a chain transfer agent with a molar ratio of 80:20:1:0.05 to 90 ℃ under the protection of nitrogen in an oil bath for 14 hours, put into an ice-water bath to terminate the reaction, and dichloromethane was used to dissolve n-hexane to precipitate, and this was repeated 3 times. After purification, P(DEGMA-OVNG) was obtained with a yield of 85%.

Embodiment 2

[0031] (1) Dissolve divinyl adipate and galactose at a molar ratio of 3:1 in 100 mL of anhydrous pyridine, add 0.5 g of alkaline protease, and react in a constant temperature water bath at 50 ° C and 200 rpm for 4 days to synthesize vinyl hexyl Galactosyl diacid (OVNG).

[0032] (2) Dissolve the synthesized OVNG and diethylene glycol dimethacrylate (DEGMA) in 2 mL of DMF, add VAZO-88 as an initiator, and add a chain transfer agent with a molar ratio of 25:75:1:0.1 at 90 ℃ under the protection of nitrogen in an oil bath for 14 hours, put into an ice-water bath to terminate the reaction, dissolve ether with methanol to precipitate, and repeat this process 3 times. After purification, P(DEGMA-OVNG) was obtained with a yield of 83%.

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Abstract

The invention relates to a method for synthesizing a galactose copolymer by adopting a RAFT method. The method comprises the following steps: dissolving adipic acid divinyl ester and galactose into a solvent; adding alkaline protease, and carrying out reaction while stirring under the condition at 40-50 DEG C for 4-5d, so as to obtain vinyl adipic acid galactose ester (OVNG); dissolving OVNG and diethylene glycol dimethacrylate (DEGMA) into the solvent; then adding an initiator and a chain transfer agent; reacting under the nitrogen protection condition of an oil bath at 90 DEG C for 10-12 hours; terminating reaction and purifying, so as to obtain the galactose copolymer. A reaction monomer is synthesized by adopting an enzymatic method, the method is strong in selectivity and high in yield, and the obtained sugar-based monomer is high in purity. The galactose copolymer is synthesized by adopting the RAFT method, the synthesis reaction is stably carried out, implosion is not generated, and the product obtained by reaction is low in molecular weight dispersing width, and the obtained copolymer has biocompatibility and low toxicity, and can be widely applied in the field of biological medicine.

Description

technical field [0001] The invention belongs to the field of preparation of galactose copolymers, in particular to a method for synthesizing galactose copolymers by RAFT method. Background technique [0002] Sugar-containing polymers have become a research hotspot in the fields of biomedicine due to their good hydrophilicity, biocompatibility and easy degradability. [0003] Rizzardo made a report on "Tailored polymers by free radical processes" at the 37th International Polymer Congress, and for the first time proposed the concept of reversible addition-fragmentation chain transfer radical polymerization (RAFT). In the traditional free radical polymerization system, the concentration of free radicals is high, and the termination reaction of free radicals is prone to occur, resulting in an uncontrollable reaction. If a special chain transfer agent with a high chain transfer constant is added to the polymerization system, the degenerate transfer between the propagating free ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/20C08F218/16C08F2/38C12P7/62
Inventor 朱利民徐慕儒权静孙衎李赫宇巫寒冰
Owner DONGHUA UNIV
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