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Method for synthesizing galactose block copolymer employing RAFT (reversible addition fragmentation chain transfer) method

A technology of block copolymer and galactose, applied in the field of preparation of galactose copolymer, can solve the problems of uncontrollable reaction, free radical termination reaction, etc., and achieve the effects of strong selectivity, low dispersion width and high purity

Inactive Publication Date: 2015-07-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 block copolymer employing RAFT (reversible addition fragmentation chain transfer) method
  • Method for synthesizing galactose block copolymer employing RAFT (reversible addition fragmentation chain transfer) method
  • Method for synthesizing galactose block copolymer employing RAFT (reversible addition fragmentation chain transfer) 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 hexyl Diacid galactosyl ester (OVAG).

[0029] (2) Dissolve diethylene glycol dimethacrylate (DEGMA) in 2 mL of DMF, add AIBN as an initiator, and add a chain transfer agent at a molar ratio of 100:1:0.2, and react for 1 h at 70°C under nitrogen protection in an oil bath , placed in an ice-water bath to terminate the reaction, and dichloromethane was used to dissolve the n-hexane precipitate, and this was repeated 3 times to obtain PDEGMA after purification.

[0030] (3) Dissolve vinyl adipate galactose (OVAG) in 2mL DMF, add AIBN as an initiator, add chain transfer agent (polyethylene glycol dimethacrylate PDEGMA), its OVAG, PDEGMA, initiator The molar ratio of 63:1:0.21 was reacted under the protection of nitrogen in an oil bath at 70°C fo...

Embodiment 2

[0032] (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 Diacid galactosyl ester (OVAG).

[0033] (2) Dissolve diethylene glycol dimethacrylate (DEGMA) in 2 mL of DMF, add AIBN as an initiator, and add a chain transfer agent at a molar ratio of 100:1:0.2, and react for 1 h at 70°C under nitrogen protection in an oil bath , placed in an ice-water bath to terminate the reaction, and dichloromethane was used to dissolve the n-hexane precipitate, and this was repeated 3 times to obtain PDEGMA after purification.

[0034] (3) Dissolve vinyl adipate galactose (OVAG) in 2mL DMF, add AIBN as an initiator, add chain transfer agent (polyethylene glycol dimethacrylate PDEGMA), its OVAG, PDEGMA, initiator The molar ratio of 80:1:0.4 was reacted under the protection of nitrogen in an oil bath at 70°C for...

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Abstract

The invention relates to a method for synthesizing a galactose block copolymer employing an RAFT (reversible addition fragmentation chain transfer) method. The method comprises the following steps: dissolving divinyl adipate and galactose into a solvent, adding alkaline protease, and carrying out reaction under stirring at 40-50 DEG C for 4-5 days, so as to obtain vinyl adipic acid galactose OVAG; dissolving macromolecular PDEGMA which is formed by polymerization of OVAG and diglycol ethylene dimethacrylate DEGMA into a solvent as a chain transfer agent; and adding an initiator AIBN, reacting in an oil bath at 70 DEG C under a nitrogen protection condition for 48 hours, terminating reaction, and purifying, so as to obtain the galactose block copolymer. A reactive monomer is synthesized by an enzyme-promoting method; the method is high in selectivity and high in yield; the obtained sugar-based monomer is high in purity; the galactose block copolymer is synthesized by the RAFT method; the synthesis reaction is stable; implosion is not caused; the molecular weight dispersing width of the product obtained by reaction is low; and the obtained copolymer has the advantages of biocompatibility and relatively low toxicity, and can be widely applied in the field of biological medicines.

Description

technical field [0001] The invention belongs to the field of preparation of galactose copolymers, in particular to a method for synthesizing galactose block 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F218/14C08F2/38
Inventor 朱利民徐慕儒权静周开春李赫宇吕瑶
Owner DONGHUA UNIV
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