1313744-91-0Relevant articles and documents
One-pot synthesis of polyrotaxane by clipping and cyclopolymerization of α,ω-diethynyl isophthalamide with pyridiniumdicarboxamide chloride
Isono, Takuya,Satoh, Toshifumi,Kakuchi, Toyoji
, p. 3184 - 3192 (2012/05/05)
The one-pot synthesis of a main chain-type polyrotaxane composed of axle molecules threaded through the macrocyclic units on the polymer main chain was achieved via the combination of cyclopolymerization and clipping procedures. The cyclopolymerization of an α,ω-diethynyl monomer bearing an isophthalamide moiety (1), which clips onto an axle component bearing a pyridiniumdicarboxamide moiety (2Cl) through a chloride anion was carried out in chloroform with the monomer concentration of 0.06 mol L-1 at 40 °C using [Rh(nbd)Cl]2/Et3N as a catalyst to afford a gel-free polymer. The resulting polymer was assigned to the main chain-type polyrotaxane with a poly(phenylacetylene) backbone (poly-3Cl) based on size exclusion chromatography and 1H NMR measurements. The diffusion-order two-dimensional NMR and circular dichroism spectra provided definitive proof of the rotaxaned architecture in the polymer. The mole fraction of the rotaxane unit in the total cyclic repeating unit was determined to be 26.3%.