Baxendale Ian R, Griffiths-Jones Charlotte M, Ley Steven V, Tranmer Geoffrey K
Innovative Technology Centre, Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK.
Chemistry. 2006 May 24;12(16):4407-16. doi: 10.1002/chem.200501400.
This article describes the design, optimisation and development of a Suzuki cross-coupling protocol mediated by an efficient palladium-encapsulated catalyst (Pd EnCat) under microwave irradiation. The methodology has been used in both batch mode for classical library preparation and in continuous-flow applications furnishing multigram quantities of material. Described is a method that uses direct focused microwave heating whilst applying an external cooling source. This enables a lower than normal bulk temperature to be maintained throughout the reaction period leading to significant improvements in the overall yield and purity of the reaction products. Additional aspects of this novel heating protocol are discussed in relation to the prolonged lifetime and enhanced reactivity of the immobilised catalyst system.
本文描述了一种由高效钯封装催化剂(Pd EnCat)介导的铃木交叉偶联反应方案在微波辐射下的设计、优化和开发。该方法已用于经典文库制备的间歇模式以及连续流应用中,可提供数克量的材料。所描述的方法是在使用外部冷却源的同时采用直接聚焦微波加热。这使得在整个反应期间能够维持低于正常的整体温度,从而显著提高反应产物的总产率和纯度。还讨论了这种新型加热方案与固定化催化剂体系延长的寿命和增强的反应活性相关的其他方面。