A One-Pot Self-Assembly Reaction To Prepare a Supramolecular Palladium(II) Cyclometalated Complex: An Undergraduate Organometallic Laboratory Experiment

Belousov-Zhabotinsky (B-Z) reaction driven polymerization-induced self-assembly (PISA), or B-Z PISA, is a novel method for the autonomous one-pot synthesis of polymer vesicles from a macroCTA (macro chain transfer agent) and monomer solution (“soup”) containing the above and the BZ reaction components. In it, the polymerization is driven (and controlled) by periodically generated radicals generated in the oscillations of the B-Z reaction. These are inhibitor/activator radicals for the polymerization. Until now B-Z PISA has only been carried out in batch reactors. In this manuscript we present the results of running the system using a continuously stirred tank reactor (CSTR) configuration which offers some interesting advantages.Indeed, by controlling the CSTR parameters we achieve reproducible and simultaneous control of the PISA process and of the properties of the oscillatory cargo encapsulated in the resulting vesicles. Furthermore, the use of flow chemistry enables a more precise morphology control and chemical cargo tuning. Finally, in the context of biomimetic applications a CSTR operation mimics more closely the open non-equilibrium conditions of living systems and their surrounding environments.

Download Full-text

Precise Synthesis and Thin Film Self-Assembly of PLLA-b-PS Bottlebrush Block Copolymers

Molecules ◽

10.3390/molecules26051412 ◽

2021 ◽

Vol 26 (5) ◽

pp. 1412

Author(s):

Eunkyung Ji ◽

Cian Cummins ◽

Guillaume Fleury

Keyword(s):

Thin Film ◽

Block Copolymers ◽

Self Assembly ◽

Ring Opening ◽

Periodic Structures ◽

One Pot ◽

Ordered Structures ◽

Carbonyl Chloride ◽

Thin Film Patterning ◽

Nanoporous Templates

The ability of bottlebrush block copolymers (BBCPs) to self-assemble into ordered large periodic structures could greatly expand the scope of photonic and membrane technologies. In this paper, we describe a two-step synthesis of poly(l-lactide)-b-polystyrene (PLLA-b-PS) BBCPs and their rapid thin-film self-assembly. PLLA chains were grown from exo-5-norbornene-2-methanol via ring-opening polymerization (ROP) of l-lactide to produce norbornene-terminated PLLA. Norbonene-terminated PS was prepared using anionic polymerization followed by a termination reaction with exo-5-norbornene-2-carbonyl chloride. PLLA-b-PS BBCPs were prepared from these two norbornenyl macromonomers by a one-pot sequential ring opening metathesis polymerization (ROMP). PLLA-b-PS BBCPs thin-films exhibited cylindrical and lamellar morphologies depending on the relative block volume fractions, with domain sizes of 46–58 nm and periodicities of 70–102 nm. Additionally, nanoporous templates were produced by the selective etching of PLLA blocks from ordered structures. The findings described in this work provide further insight into the controlled synthesis of BBCPs leading to various possible morphologies for applications requiring large periodicities. Moreover, the rapid thin film patterning strategy demonstrated (>5 min) highlights the advantages of using PLLA-b-PS BBCP materials beyond their linear BCP analogues in terms of both dimensions achievable and reduced processing time.

Download Full-text

Chiroptical Probing of Lanthanide-Directed Self-Assembly Formation Using btp Ligands Formed in One-Pot Diazo-Transfer/Deprotection Click Reaction from Chiral Amines

Chemistry - A European Journal ◽

10.1002/chem.201504257 ◽

2015 ◽

Vol 22 (2) ◽

pp. 486-490 ◽

Cited By ~ 27

Author(s):

Joseph P. Byrne ◽

Miguel Martínez-Calvo ◽

Robert D. Peacock ◽

Thorfinnur Gunnlaugsson

Keyword(s):

Self Assembly ◽

Click Reaction ◽

Chiral Amines ◽

One Pot

Download Full-text

One-pot synthesis of a TiO2–CdS nano-heterostructure assembly with enhanced photocatalytic activity

RSC Advances ◽

10.1039/c5ra04733a ◽

2015 ◽

Vol 5 (44) ◽

pp. 34942-34948 ◽

Cited By ~ 10

Author(s):

Sayantan Mazumdar ◽

Aninda J. Bhattacharyya

Keyword(s):

Titanium Dioxide ◽

Photocatalytic Activity ◽

Cadmium Sulfide ◽

Self Assembly ◽

Cost Effective ◽

One Pot ◽

One Pot Synthesis ◽

Cost Effective Method

An unprecedented morphology of a titanium dioxide (TiO2) and cadmium sulfide (CdS) self-assembly obtained using a ‘truly’ one-pot and highly cost effective method with a multi-gram scale yield is reported here.

Download Full-text

PhotoATRP Induced Self-Assembly (PhotoATR-PISA) Enables Simplified Synthesis of Responsive Polymer Nanoparticles in One-Pot

10.26434/chemrxiv.12988559 ◽

2020 ◽

Author(s):

Ali Shahrokhinia ◽

Randall Scanga ◽

Priyanka Biswas ◽

James Reuther

Keyword(s):

Self Assembly ◽

Glycidyl Methacrylate ◽

Uv Light ◽

Copper Catalyst ◽

Crosslinking Agent ◽

Polymer Nanoparticles ◽

One Pot ◽

Responsive Polymer ◽

Catalyst Systems ◽

First Time

ABSTRACT: Photo-controlled atom transfer radical polymerization (PhotoATRP) was implemented, for the first time, to accomplish polymerization induced self-assembly (PISA) mediated by UV light (λ = 365 nm) using ppm levels (ca. < 20 ppm) of copper catalyst at ambient temperature. Using CuIIBr2/tris(pyridin-2-ylmethyl)amine (TPMA) catalyst systems, PISA was per-formed all in one-pot starting from synthesis of solvophilic poly(oligo(ethylene oxide) methyl ether methacrylate) (POEGMA) blocks to core-crosslinked nanoparticles (NPs) utilizing poly(glycidyl methacrylate) (PGMA) and N,N-cystamine bismethacrylamide (CBMA) as the solvophobic copolymer and crosslinking agent, respectively. Sequential chain-extensions were performed for PGMA demonstrating capabilities for accessing multi-block copolymers with temporal control via switching the UV light on and off. Further, core-crosslinking of PISA nanoparticles was performed via the slow incorporation of the CBMA enabling one-pot crosslinking during the PISA process. Finally, the disulfide installed in the CBMA core-crosslinks allowed for the stimuli-triggered dissociation of nanoparticles using DL-dithiothreitol at acidic pH.

Download Full-text

One-pot synthesis of noble metal nanoparticles and their ordered self-assembly nanostructures

Soft Matter ◽

10.1039/c2sm07004a ◽

2012 ◽

Vol 8 (14) ◽

pp. 3743 ◽

Cited By ~ 11

Author(s):

Dharmesh Varade ◽

Kazutoshi Haraguchi

Keyword(s):

Metal Nanoparticles ◽

Noble Metal ◽

Self Assembly ◽

Noble Metal Nanoparticles ◽

One Pot ◽

One Pot Synthesis

Download Full-text

A facile one-pot self-assembly approach to incorporate SnOx nanoparticles in ordered mesoporous carbon with soft templating for fuel cells

Nanotechnology ◽

10.1088/0957-4484/25/13/135403 ◽

2014 ◽

Vol 25 (13) ◽

pp. 135403 ◽

Cited By ~ 5

Author(s):

Yingqiang Huang ◽

Zhicheng Zhai ◽

Zhigang Luo ◽

Yingju Liu ◽

Zhurong Liang ◽

...

Keyword(s):

Fuel Cells ◽

Self Assembly ◽

Mesoporous Carbon ◽

Ordered Mesoporous Carbon ◽

One Pot ◽

Ordered Mesoporous ◽

Soft Templating

Download Full-text

Oxidation-responsive micelles by a one-pot polymerization-induced self-assembly approach

Polymer Chemistry ◽

10.1039/c7py01859b ◽

2018 ◽

Vol 9 (13) ◽

pp. 1593-1602 ◽

Cited By ~ 23

Author(s):

Fabian H. Sobotta ◽

Franziska Hausig ◽

Dominic O. Harz ◽

Stephanie Hoeppener ◽

Ulrich S. Schubert ◽

...

Keyword(s):

Self Assembly ◽

Raft Polymerization ◽

Assembly Process ◽

Carrier System ◽

One Pot ◽

System P

Combining a sequential, one-pot RAFT polymerization with the polymerization-induced self-assembly process results in a versatile oxidation-responsive carrier system.

Download Full-text

Synthesis and Morphological Control of Biocompatible Fluorescent/Magnetic Janus Nanoparticles Based on the Self-Assembly of Fluorescent Polyurethane and Fe3O4 Nanoparticles

Polymers ◽

10.3390/polym11020272 ◽

2019 ◽

Vol 11 (2) ◽

pp. 272 ◽

Cited By ~ 3

Author(s):

Botian Li ◽

Wei Shao ◽

Yanzan Wang ◽

Da Xiao ◽

Yi Xiong ◽

...

Keyword(s):

Self Assembly ◽

Laser Scanning ◽

Particle Morphology ◽

Confocal Laser Scanning Microscope ◽

Confocal Laser ◽

Magnetic Composite ◽

Fluorescent Properties ◽

One Pot ◽

Janus Nanoparticles ◽

Nano Fe3o4

Functionalized Janus nanoparticles have received increasing interest due to their anisotropic shape and the particular utility in biomedicine areas. In this work, a simple and efficient method was developed to prepare fluorescent/magnetic composite Janus nanoparticles constituted of fluorescent polyurethane and hydrophobic nano Fe3O4. Two kinds of fluorescent polyurethane prepolymers were synthesized by the copolymerization of fluorescent dye monomers, and the fluorescent/magnetic nanoparticles were fabricated in one-pot via the process of mini-emulsification and self-assembly. The nanostructures of the resulting composite nanoparticles, including core/shell and Janus structure, could be controlled by the phase separation in assembly process according to the result of transmission electron microscopy, whereas the amount of the nonpolar segments of polyurethane played an important role in the particle morphology. The prominent magnetic and fluorescent properties of the Janus nanoparticles were also confirmed by vibrating magnetometer and confocal laser scanning microscope. Furthermore, the Janus nanoparticles featured excellent dispersity, storage stability, and cytocompatibility, which might benefit their potential application in biomedical areas.

Download Full-text