Szczepaniak Grzegorz, Urbaniak Katarzyna, Wierzbicka Celina, Kosiński Krzysztof, Skowerski Krzysztof, Grela Karol
Biological and Chemical Research Centre, Faculty of Chemistry, University of Warsaw, Żwirki i Wigury 101, 02-089, Warsaw, Poland.
Apeiron Synthesis, Duńska 9, 54-427, Wrocław, Poland.
ChemSusChem. 2015 Dec 21;8(24):4139-48. doi: 10.1002/cssc.201500784. Epub 2015 Nov 11.
Three isocyanides containing a tertiary nitrogen atom were investigated for use as small-molecule ruthenium scavenging agents in the workup of olefin metathesis reactions. The proposed compounds are odorless, easy to obtain, and highly effective in removing metal residues, sometimes bringing the metal content below 0.0015 ppm. The most successful of the tested compounds, II, performs very well, even with challenging polar products. The performance of these scavengers is compared and contrasted with other known techniques, such as silica gel filtration and the use of self-scavenging catalysts. As a result, a new hybrid purification method is devised, which gives better results than using either a self-scavenging catalyst or a scavenger alone. Additionally, isocyanide II is shown to be a deactivating (reaction quenching) agent for olefin metathesis and superior to ethyl vinyl ether.
研究了三种含有叔氮原子的异腈类化合物,用于烯烃复分解反应后处理中作为小分子钌清除剂。所提出的化合物无味、易于获得,并且在去除金属残留物方面非常有效,有时能使金属含量降至0.0015 ppm以下。测试的化合物中最成功的II,即使对于具有挑战性的极性产物也表现良好。将这些清除剂的性能与其他已知技术进行了比较和对比,如硅胶过滤和使用自清除催化剂。结果,设计了一种新的混合纯化方法,其效果优于单独使用自清除催化剂或清除剂。此外,异腈II被证明是烯烃复分解的失活(反应淬灭)剂,且优于乙基乙烯基醚。