Sequestration of Ruthenium Residues via Efficient Fluorous-enyne Termination.

Sequestration of Ruthenium Residues via Efficient Fluorous-enyne Termination.
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通过有效的氟烯炔封端封存钌残留物。

DOI:
10.1039/d3py00456b
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发表时间:
2023
期刊:
影响因子:
4.6
通讯作者:
Gutekunst,WillR
Gutekunst,WillR
中科院分区:
化学2区
文献类型:
--
作者:
Sui,Xuelin;Wang,Chenxiao;Gutekunst,WillR

文献摘要

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创造没有金属污染的聚合物仍然是基于复分解的聚合技术的重大挑战,并且在生物医学和电子应用中具有复杂的应用。该通讯报道了一种通过设计包含氟标签的用于复分解聚合的烯炔终止剂来去除钌副产物的新方法。当活性聚合物链与烯炔发生反应时,钌中心被捕获为稳定的硫螯合络合物,该络合物可以在通过含氟滤芯单次过滤后被有效去除。通过 ICP-MS 测定的钌残留物含量被发现取决于单体结构、洗脱溶剂和目标聚合度。对于大多数检查样品,钌残留量已降至低 ppm 水平(4-75 ppm),并且还提高了最终材料的热稳定性。这是从复分解聚合产物中去除钌残留物的最有效的单一方法。
The creation of polymers without metal contamination remains a significant challenge for metathesis-based polymerization techniques and has complicated applications in biomedical and electronic applications. This communication reports a new approach for the removal of ruthenium byproducts through the design of an enyne terminator for metathesis polymerization that contains a fluorous tag. Upon reaction of a living polymer chain with the enyne, the ruthenium center is captured as a stable sulfur-chelated complex that can be efficiently removed after a single filtration through a fluorous cartridge. Levels of ruthenium residues as determined by ICP-MS were found to depend on the monomer structure, eluting solvent, and the degree of polymerization targeted. Ruthenium residues were minimized to low ppm levels (4–75 ppm) for most samples examined and also led to the improved thermal stability of the final materials. This represents the most efficient single method for removal of ruthenium residues from metathesis polymerization products.