Design and Precise Synthesis of Thermoresponsive by Keita Fuchise

By Keita Fuchise

In this thesis, the writer describes flexible and easy-to-use easy methods to keep an eye on the homes of thermoresponsive polyacrylamides via constructing novel man made equipment for end-functionalized poly(N-isopropylacrylamide) (PNIPAM) and block copolymers of poly(N,N-diethylacrylamide) (PDEAA). The synthesis of varied urea end-functionalized PNIPAMs used to be completed through the atom move radical polymerization (ATRP) and the clicking response. The part transition temperature of PNIPAM in water was once managed counting on the power of the hydrogen bonding of the urea teams brought on the chain finish of the polymer. Novel dwelling polymerization tools for N,N-dimethylacrylamide and N,N-diethylacrylamide have been constructed by way of staff move polymerization (GTP) utilizing a powerful Brønsted acid as a precatalyst and an amino silyl enolate as an initiator. This technique enabled the correct synthesis of PDEAA and its block copolymers—namely, thermoresponsive amphiphilic block copolymers and double-hydrophilic block copolymers.

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0 °C min−1. 14 Dynamic Light Scattering Measurement The hydrodynamic diameter (Dh) and size distribution for the polymer aggregated in an aqueous solution were determined by dynamic light scattering (DLS) at the fixed scattering angle of 90°. 20 mg mL−1). 45 μm membrane filter. The measurement was carried out after the sample stood for at least 1 h at 25 °C. The Dh and particle size distribution were calculated by the CONTIN analysis. 20 mg mL−1) was stirred for 72 h at room temperature in order to reach thermodynamic equilibrium.

The group transfer polymerization (GTP) for acrylamide monomers was expected to provide excellent control of the polymerization in comparison to the existing controlled/living polymerizations and become a robust method to precisely synthesize thermoresponsive polyacrylamides and their block copolymers, namely thermoresponsive amphiphilic block copolymers and double-hydrophilic block copolymers. The outline of this thesis is as follows. 4 Graphical abstract of Chap. 4. A series of PNIPAMs with different diphenylurea groups at the chain end (X-PhNH-CO-NH-Ph-trz-PNIPAM: X = H, OCH3, CH3, NO2, Cl, and CF3) were synthesized by the ATRP and the CuAAC.

20. Anal. 84. 7 mmol) were added to a round bottom flask. The flask was capped with a septum, and purged with argon. 95 mol L−1) were then sequentially added. The reaction mixture was stirred for 4 h at room temperature. The polymerization was quenched by exposure to air. 1 %). The reaction mixture was diluted with THF and passed through a short column of silica gel to remove the copper complex. The obtained solution was dialyzed using a cellophane tube (Spectra/Por® 6 Membrane; MWCO: 1000) in methanol and finally reprecipitated from THF into hexane to provide the azido end-functionalized PNIPAM (2) as a white solid.

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