Polypeptide and polytetrahydrofuran graft copolymer and preparation method thereof
A technology of polytetrahydrofuran and graft copolymers, which is applied in the field of polymer material synthesis and preparation, can solve the problems of graft copolymers that have not been reported, increase the moisture resistance strength of copolymers, affect the efficiency of block copolymerization, etc., and achieve designable Strong resistance, moisture resistance, crystallization self-reinforcement, excellent biocompatibility
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Embodiment 1
[0028] Poly(γ-benzyl-L-glutamate)-g-polytetrahydrofuran graft copolymer
[0029] A: Under nitrogen protection, dissolve 4.0g of γ-benzyl ester-L-glutamic acid (BLG) in 40mL of tetrahydrofuran (THF), add 2.0g of triphosgene, and react at 60°C for 2 hours to generate γ- Benzyl ester-L-glutamic acid-N-carboxyl internal anhydride (BLG-NCA) was precipitated with petroleum ether, filtered and dried to obtain the product with a yield of 33%. Dissolve 2.0 g of BLG-NCA in N, N-dimethylformamide, add 40 mg of triethylamine, react at 25 ° C for 6 hours, precipitate with methanol, and then dry in vacuo to obtain poly(γ-benzyl- L-glutamic acid ester), namely PBLG, the yield is 78%.
[0030] B: Under the protection of nitrogen, add 0.2mL methyl trifluoromethanesulfonate to 10mL solution containing THF and chloroform ([THF]=6.2mol / L), trigger THF to carry out living ring-opening polymerization at 20°C After 10 minutes, a single-ended polytetrahydrofuran active chain solution was obtained. ...
Embodiment 2
[0033] Poly(γ-benzyl-L-glutamate)-g-polytetrahydrofuran graft copolymer
[0034] A: Same as A in Example 1.
[0035] B: Same as B in Example 1, except that bulk polymerization is used.
[0036] C: Add 0.3 mL of the polytetrahydrofuran active chain solution of step B to 20 mL of the above PBLG in chloroform ([PBLG]=3.6 mmol / L) under stirring conditions, and react at 20° C. for 30 minutes. The obtained product was purified by chloroform and tetrahydrofuran solvents in sequence, and the purified product was vacuum-dried at a constant temperature of 40° C. for 18 hours to obtain 0.24 g of graft copolymer PBLG-g-PTHF. The grafting rate is 5%, and the M of the main chain PBLG n M of 2300, branched chain PTHF n for 1100.
Embodiment 3
[0038] Poly(γ-benzyl-L-glutamate)-g-polytetrahydrofuran graft copolymer
[0039] A: Same as A in Example 1.
[0040] B: Just change the addition amount of methyl trifluoromethanesulfonate to 0.3mL, and other conditions are the same as B in Example 1.
[0041] C: Under stirring conditions, add 4 mL of the polytetrahydrofuran living chain solution of step B to 20 mL of the above PBLG in chloroform ([PBLG]=3.6 mmol / L), and react at 20° C. for 30 minutes. The obtained product was purified by chloroform and tetrahydrofuran solvents in sequence, and the purified product was vacuum-dried at constant temperature at 40° C. for 18 hours to obtain 1.2 g of graft copolymer PBLG-g-PTHF. The grafting rate was 81%, and the M of the main chain PBLG n M of 2300, branched chain PTHF n for 700.
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Abstract
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