Convenient multigram synthesis of monodisperse oligo(ethylene glycols): effective reaction monitoring by infrared spectroscopy using an attenuated total reflection fibre optic probe
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- 作者：Daniel Lumpi ; Christian Braunshier ; Christian Hametner ; Ernst Horkel ; Bernhard Zachhuber ; Bernhard Lendl ; Johannes Frö ; hlich
- 关键词：Monodisperse OEG PEG ; Trityl cleavage ; Oligo(ethylene glycols) ; In situ reaction monitoring ; ATR-IR-sensor spectroscopy
- 刊名：Tetrahedron Letters
- 出版年：2009
- 出版时间：25 November 2009
- 年：2009
- 卷：50
- 期：47
- 页码：6469-6471
- 全文大小：188 K
文摘
A convenient approach for the synthesis of monodisperse oligo(ethylene glycols) up to 12 units is described. A novel cleavage protocol replacing laborious hydrogenolysis is introduced to achieve a fast, inexpensive and widely applicable procedure. In addition to the synthetic part, Fourier transform infrared (FTIR) spectroscopy using a fibre optic attenuated total reflection (ATR) sensor was applied to monitor the formation of sensitive key intermediates, resulting in optimized reaction times. By applying this in-line technique, the possibility of real-time analysis under inert conditions was impressively demonstrated.