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Method for synthesizing glucose-containing segmented copolymer by RAFT (Reversible Addition Fragmentation chain Transfer) method

A technology of block copolymer and glucose, applied in the field of synthesizing glucose-containing block copolymer by RAFT method, can solve the problems of uncontrollable reaction, free radical termination reaction, etc., and achieve the effect of low dispersion width and low toxicity

Inactive Publication Date: 2014-04-02
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 glucose-containing segmented copolymer by RAFT (Reversible Addition Fragmentation chain Transfer) method
  • Method for synthesizing glucose-containing segmented copolymer by RAFT (Reversible Addition Fragmentation chain Transfer) method
  • Method for synthesizing glucose-containing segmented copolymer by RAFT (Reversible Addition Fragmentation chain Transfer) method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Dissolve 12g of divinyl adipate and 4g of glucose in 100mL of anhydrous pyridine, add 0.5g of alkaline protease, and react in a constant temperature water bath at 50°C and 210rpm for 4 days to synthesize vinyl adipate glucose ester ( OVAG), the yield was 67%.

[0027] (2) Dissolve 0.58g of synthesized OVAG and 1.78g of N-isopropylacrylamide (NIPAm) in 2mL of DMF, add 1.5mg of AIBN as an initiator, add 63mg of chain transfer agent, and react for 12h at 70°C under the protection of nitrogen in an oil bath , put into an ice-water bath to terminate the reaction, dissolve the ether precipitate with methanol, repeat this process 3 times, and obtain P(NIPAm-OVAG) after purification with a yield of 82%.

[0028] (3) Dissolve 0.3g of synthesized P(NIPAm-OVAG) and 0.216g of N-isopropylacrylamide (NIPAm) in 1mL of DMF, add 0.25mg of AIBN as an initiator, and react for 7h under the protection of nitrogen in an oil bath at 70°C. The reaction was terminated by putting in liquid ...

Embodiment 2

[0030] (1) Dissolve 12g of divinyl adipate and 6g of glucose in 100mL of anhydrous pyridine, add 0.5g of alkaline protease, and react in a constant temperature water bath at 50°C and 200rpm for 4 days to synthesize vinyl adipate glucose ester ( OVAG), the yield was 61%.

[0031] (2) Dissolve 0.58g of synthesized OVAG and 0.80g of N-isopropylacrylamide (NIPAm) in 2mL of DMF, add 0.75mg of AIBN as an initiator, add 32mg of chain transfer agent, and react for 12h under the protection of nitrogen in an oil bath at 70°C , put into an ice-water bath to terminate the reaction, dissolve the ether precipitate with methanol, repeat this process 3 times, and obtain P(NIPAm-OVAG) after purification with a yield of 80%.

[0032] (3) Dissolve 0.3 g of synthesized P(NIPAm-OVAG) and 0.19 g of N-isopropylacrylamide (NIPAm) in 1 mL of DMF, add 0.23 mg of AIBN as an initiator, and react for 6 h at 70 °C under the protection of nitrogen in an oil bath. The reaction was terminated by putting in l...

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Abstract

The invention relates to a method for synthesizing glucose-containing segmented copolymer by using a RAFT method. The method comprises the following steps of dissolving diviny adipate and glucose in a solvent, adding alkaline protease, reacting for 4-5d while stirring at 40-50 DEG C, thereby obtaining the 6-O-vinyl adipate-D-glucose (OVAG); dissolving OVAG and N-isopropyl acrylamide (NIPAm) in a solvent, adding an initiator and a chain transfer agent, reacting for 10-12h at 60-70 DEG C, terminating the reaction, purifying to obtain P(NIPAm-OVAG); dissolving the P(NIPAm-OVAG) into solvent, adding NIPAm and an initiator, reacting for 6-10h at 60-70 DEG C, terminating the reaction, purifying, thereby obtaining product. In the method, reaction is steady, implosion is avoided, and reaction product has low molecular weight distribution width; the segmented copolymer obtained from reaction has biocompatibility, is low-toxicity, and can be widely used in the biological medicine field.

Description

technical field [0001] The invention belongs to the field of sugar-containing polymers, in particular to a method for synthesizing glucose-containing block copolymers by a 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 Conference, 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 propagat...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F220/54C08F218/16C08F2/38C12P19/44
Inventor 朱利民孙衎权静巫寒冰徐慕儒
Owner DONGHUA UNIV
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