Worldwide Research and Development, Pfizer Inc., Eastern Point Road, Groton, Connecticut 06340, USA.
Org Lett. 2013 Sep 6;15(17):4342-5. doi: 10.1021/ol4018134. Epub 2013 Aug 12.
High-yielding Heck reactions are demonstrated using 0.05 mol % Pd(OAc)2 without phosphine ligands. These reactions are run in a mesoscale flow reactor which allows precise control of reaction times and temperatures. Profiling yield and selectivity versus Pd loading shows 500 ppm to be optimal for aryl iodides; higher loadings favor side reactions caused by Pd(II) species. Aryl halides are examined via concise Design of Experiment to expand the scope and optimize conditions.
高产 Heck 反应在无需膦配体的情况下使用 0.05 mol% 的 Pd(OAc)2 进行。这些反应在中试规模的流动反应器中进行，可精确控制反应时间和温度。对产率和选择性与 Pd 负载量的关系进行分析表明，对于芳基碘化物而言，500 ppm 为最佳负载量；更高的负载量有利于由 Pd(II)物种引起的副反应。通过简洁的实验设计考察了芳基卤化物，以扩展反应范围并优化条件。
