Intensive Cycloalkyl-Fused Pyridines for Aminopyridyl-Zinc-Heteroimidazoles Achieving High Efficiency toward the Ring-Opening Polymerization of Lactides

环烷基稠合吡啶类化合物高效催化氨基吡啶基锌杂咪唑开环聚合反应,实现高效聚合

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Abstract

The model precatalyst sp(3)- and sp(2)-N dinitrogen-coordinated zinc-heteroimidazole has been used as an efficient catalyst for the ring-opening polymerization of cyclic esters. Subsequent to our exceptional active 5,6,7-trihydroquinolin-8-amine-zinc catalysts for the ring-opening polymerization (ROP) of ε-caprolactone, various pyridine-fused cycloalkanones (ring size from five to eight) are developed for the correspondent fused amine-pyridine derivatives and their zinc-heteroimidazole chloride complexes Zn1-Zn8 (LZnCl(2)) bearing N-diphenylphosphinoethyl pendants. Activated with two equivalents of LiN(SiMe(3))(2), the title zinc complexes efficiently promote the ROP of L-lactide (L-LA) in situ; among them, Zn4/2Li(NSiMe(3))(2) catalyzed 500 equivalent L-LA at 80 °C with 92% conversion in 5 min (TOF: 5520 h(-1)). Under the same conditions, the catalytic efficiency for the ROP of rac-LA by Zn1-Zn8/2Li(NSiMe(3))(2) was slightly lower than that for L-LA (highest TOF: 4440 h(-1)). In both cases, cyclooctyl-fused pyridyl-zinc complexes exhibited higher activity than others, while the cycloheptyl-fused zinc complexes showed the lowest activity. The microstructure analysis of the polymers showed they possessed a linear structure capped with CH(3)O as major and cyclic structure as minor. In this work, all the ligands and zinc complexes were well characterized by (1)H/(13)C/(31)P NMR, FT-IR spectroscopy as well as elemental analysis.

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