Department of Chemistry, Faculty of Science, Hokkaido University, Sapporo 060-0810, Japan.
J Am Chem Soc. 2010 Jan 20;132(2):879-89. doi: 10.1021/ja9092264.
Reactions between acyclic (E)-allylic acetates and arylboronic acids in the presence of a palladium catalyst prepared from Pd(OAc)(2), phenanthroline (or bipyridine), and AgSbF(6) (1:1.2:1) proceeded with excellent gamma-selectivity to afford allyl-aryl coupling products with E-configuration. The reactions of alpha-chiral allylic acetates took place with excellent alpha-to-gamma chirality transfer with syn stereochemistry to give allylated arenes with a stereogenic center at the benzylic position. The reaction tolerated a broad range of functional groups in both the allylic acetates and the arylboronic acids. Furthermore, gamma-arylation of cinnamyl alcohol derivatives afforded gem-diarylalkane derivatives containing an unconjugated alkenic substituent. The synthetic utility of this method was demonstrated by its utilization in an efficient synthesis of (+)-sertraline, an antidepressant agent. The observed gamma-regioselectivity and E-1,3-syn stereochemistry were rationalized based on a Pd(II) mechanism involving transmetalation between a cationic mono(acyloxo)palladium(II) complex and arylboronic acid, and directed carbopalladation followed by syn-beta-acyloxy elimination. The results of stoichiometric reactions of palladium complexes related to possible intermediates were fully consistent with the proposed mechanism.
(E)-烯丙基乙酸酯与芳基硼酸在 Pd(OAc)(2)、菲咯啉(或联吡啶)和 AgSbF(6)(1:1.2:1)组成的钯催化剂存在下反应,具有极好的γ-选择性,生成 E 构型的烯丙基-芳基偶联产物。α-手性烯丙基乙酸酯的反应以极好的α到γ的手性转移和 syn 立体化学进行,生成苄位具有手性中心的烯丙基芳基化合物。该反应在烯丙基乙酸酯和芳基硼酸中都能容忍广泛的官能团。此外,肉桂醇衍生物的γ-芳基化反应得到含有非共轭烯属取代基的双芳基烷烃衍生物。该方法的合成实用性通过其在抗抑郁药(+)-舍曲林的高效合成中的应用得到了证明。观察到的γ-区域选择性和 E-1,3-syn 立体化学可以根据涉及阳离子单(烷氧基)钯(II)配合物和芳基硼酸之间的转金属化以及随后的 syn-β-烷氧基消除的 Pd(II)机理来解释。与可能的中间体相关的钯配合物的化学计量反应的结果与所提出的机理完全一致。