Peptide-like monomer as well as polymer and application thereof
A technology for polymers and degradable polymers, which is applied in the field of biomedical materials, can solve the problems that the substituent groups cannot be functionally modified, hinder the application of polymer peptide polymers, etc., and achieve rich types, simple and fast synthesis methods, and mild synthesis conditions Effect
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Embodiment 1
[0050] Embodiment 1: the preparation of azidoalkyl alcohol compound
[0051] Bromopropanol (1.38g, 0.01mol) and sodium azide (0.975g, 0.015mol) were weighed and dissolved in N,N-dimethylformamide (DMF), and reacted at 90°C for 12h under nitrogen protection. After the reaction, the solution was cooled to room temperature, diluted with a certain amount of water, and the aqueous layer was washed with a large amount of ether to extract the product, the ether solution was collected and washed with anhydrous NaSO 4 Dry overnight, filter and concentrate the crude product to remove residual DMF organic solvent by column chromatography, developing agent is ethyl acetate:petroleum ether=1:5, the colorless liquid obtained is the product azidopropanol, yield It was 0.873g, and the yield was 86.4%. Using the same procedure, azidohexanol (0.69 g, 89.2%) and azidedecanol (0.98 g, 91.7%) can be prepared.
[0052]
[0053] Azidopropanol (m=1) 1 H NMR (CDCl 3 ):δ=3.74(-CH 2 N 3 ),3.4...
Embodiment 2
[0057] Embodiment 2: Preparation of N-hydroxyalkyl-β-alanine carboxylic acid anhydride compound
[0058] Dissolve azidopropanol and succinic anhydride in hexafluoroisopropanol (HFIP) at a molar ratio of 1.2:1, slowly add 1.1 equivalents of boron trifluoride ether as a catalyst, and react the reaction solution in a glove box for 6 hours at low temperature. There will be more N in the early stage of the reaction 2 Therefore, it is necessary to continuously rotate the piston to remove the gas in the system. After the reaction, anhydrous pyridine equivalent to boron trifluoride ether was slowly added dropwise to the reaction liquid to neutralize the acid in the system, and the stirring was continued for 1 h. After the reaction solution is concentrated, it is purified and separated by column chromatography in the glove box. The ratio of developing agent ethyl acetate / petroleum ether is 1:2, and the collected solution is concentrated to prepare N-hydroxypropyl-β-alanine carboxyli...
Embodiment 3
[0068] Example 3: Preparation of Polypeptide Poly(N-hydroxyundecyl-β-alanine) (PC11OHNNCA)
[0069] Dissolve a certain amount of monomer N-hydroxyl undecyl-β-alanine carboxylic anhydride in a certain amount of dry DMF solvent in the glove box, then add benzylamine initiator in the system (initiator dose is determined according to the theoretical design molecular weight , such as the design degree of polymerization is 50, the amount of benzylamine is 1 / 50 of the molar amount of the monomer), and placed in an oil bath at 50° C. under the protection of argon for sealing reaction for 24 hours. After the reaction, the reaction solution was returned to room temperature, and was repeatedly settled three times in a large amount of anhydrous ether, and then dried in vacuum to obtain the polymer product. The synthesis methods of other types of clustered peptides are similar to the above operations.
[0070]
[0071] Poly(N-hydroxyundecyl-β-alanine) (PC11OHNNCA) NMR: 1 H NMR (CDCl...
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