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评价一种用于反应筛选、优化和合成的商业填充床流动加氢器。

Evaluation of a commercial packed bed flow hydrogenator for reaction screening, optimization, and synthesis.

机构信息

Medicinal Chemistry Research Technology, Department of Chemistry Research and Discovery, Amgen, Inc., One Amgen Center Drive, Thousand Oaks, CA 91320, USA.

出版信息

Beilstein J Org Chem. 2011;7:1141-9. doi: 10.3762/bjoc.7.132. Epub 2011 Aug 22.

Abstract

The performance of the ThalesNano H-Cube(®), a commercial packed bed flow hydrogenator, was evaluated in the context of small scale reaction screening and optimization. A model reaction, the reduction of styrene to ethylbenzene through a 10% Pd/C catalyst bed, was used to examine performance at various pressure settings, over sequential runs, and with commercial catalyst cartridges. In addition, the consistency of the hydrogen flow was indirectly measured by in-line UV spectroscopy. Finally, system contamination due to catalyst leaching, and the resolution of this issue, is described. The impact of these factors on the run-to-run reproducibility of the H-Cube(®) reactor for screening and reaction optimization is discussed.

摘要

泰雷兹纳诺 H-Cube(®)的性能评估,商业填充床流动氢化器,在小规模反应筛选和优化的背景下进行。通过 10% Pd/C 催化剂床,使用模型反应将苯乙烯还原为乙苯,检查在各种压力设置下、连续运行中和使用商业催化剂盒的性能。此外,通过在线 UV 光谱法间接测量氢气流量的一致性。最后,描述了催化剂浸出引起的系统污染以及解决此问题的方法。讨论了这些因素对 H-Cube(®)反应器用于筛选和反应优化的运行重复性的影响。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/eae0/3170201/fe0de2de2d7e/Beilstein_J_Org_Chem-07-1141-g009.jpg

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