Department of Chemistry and Biochemistry, Florida State University, Tallahassee, Florida 32306, USA.
Org Lett. 2013 Mar 1;15(5):996-9. doi: 10.1021/ol303442m. Epub 2013 Feb 13.
It is demonstrated that homogeneous N-heterocyclic carbene-copper(I)-chloride complexes can be prepared continuously by flowing NHC precursors through a packed bed of solid Cu(2)O suspended in molecular sieves. The method enables the synthesis of a wide range of complexes including those that are challenging to prepare using standard approaches. Our strategy enables both sustained output of complex production for long-term catalytic reactions (greater than 5 h) and for generation of gram quantities for storage (greater than 1 g of complex in ~16 min).
研究表明，通过将 N-杂环卡宾（NHC）前体流经固定在分子筛中的氧化铜（Cu2O）颗粒床，可连续制备均相 N-杂环卡宾-铜（I）-氯化物配合物。该方法可合成多种配合物，包括那些使用标准方法难以制备的配合物。我们的策略不仅可以实现复杂化合物的持续生产，以满足长期催化反应的需要（大于 5 小时），而且可以实现克级规模的化合物的生产（在 16 分钟左右可获得约 1 克的配合物）。
