Block copolymer, its preparation method and hydrogel and its preparation method
A technology of block copolymer and hydrogel, which is applied in the field of its preparation, block copolymer, hydrogel and its preparation, can solve the problem of non-degradable, difficult to achieve gel reversible into solution state, polymerized monomer Toxicity and other issues, to achieve the effect of good fluidity, good biodegradability, good biocompatibility
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[0043] The application also provides a kind of preparation method of block copolymer, comprises the following steps:
[0044] One of the end-aminated polyethylene glycol monomethyl ether with formula (IV) structure and the end-amination polyethylene glycol with formula (V) structure and γ-ethoxydiethylene glycol- L-glutamate-N-carboxylic acid internal anhydride is polymerized to obtain a block copolymer;
[0045]
[0046] Among them, 10≤m≤227; 10≤n≤226.
[0047] According to the present invention, in order to make the polyethylene glycol monomethyl ether in the block polymer and one of the polyethylene glycol and the γ-ethoxydiethylene glycol-L-glutamic acid Ester-N-carboxylic acid internal anhydride reaction is sufficient, and the preparation process of described block copolymer is specifically:
[0048] One of the aminated polyethylene glycol monomethyl ether having the structure of formula (IV) and the aminated polyethylene glycol having the structure of formula (V) is d...
Embodiment 1
[0087] Preparation of γ-Ethoxydiethylene Glycol-L-Glutamate-N-Carboxylidene Anhydride:
[0088] Mix and stir 30gL-glutamic acid and 120ml diethylene glycol ethyl ether, and add 18ml concentrated sulfuric acid dropwise thereto under stirring conditions, in the presence of concentrated sulfuric acid and stirring conditions, L-glutamic acid and diethylene glycol Ether was esterified, and the reaction time was 24h. After completion of the reaction, neutralize the resulting reaction solution with a mixed solution of 97ml triethylamine and 300ml isopropanol, then centrifuge, recrystallize and dry the resulting mixed solution to obtain γ-ethoxydiethylene glycol-L- Glutamate, the yield was 46.6%.
[0089] Take 20 g of the obtained γ-ethoxydiethylene glycol-L-glutamate and put it into 150 ml of tetrahydrofuran, slowly add 11 g of bis(trichloromethyl)carbonate, the reaction temperature is 50°C, and the reaction time is preferably 0.5 h. After the reaction, the reaction solution was p...
Embodiment 2
[0091] Azeotrope 1.5 g of aminated polyethylene glycol monomethyl ether with a number average molecular weight of 750 and 60 mL of anhydrous toluene at 130 ° C for 2 h to remove water, then drain the remaining toluene under reduced pressure, and dissolve the obtained solid in In 20 mL of dry N,N-dimethylformamide, the first solution was obtained; 4.05 g of γ-ethoxydiethylene glycol-L-glutamate-N-carboxylate anhydride was dissolved in 40 mL of dry In N,N-dimethylformamide, the second solution was obtained; in a nitrogen atmosphere, the first solution was mixed with the second solution, and the reaction was stirred and reacted at 40°C for 72h under nitrogen protection conditions. After the reaction was completed, use Diethyl ether was settled, suction filtered, and dried to obtain a polyethylene glycol monomethyl ether-poly(γ-ethoxydiethylene glycol-L-glutamate) block copolymer having a structure of formula (VI).
[0092] The block copolymer obtained above is carried out nuclear...
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