Roy and Diana Vagelos Laboratories, Penn/Merck Laboratory for High-Throughput Experimentation, Department of Chemistry, University of Pennsylvania, 231 South 34th Street, Philadelphia, Pennsylvania 19104-6323, USA.
J Am Chem Soc. 2011 Dec 21;133(50):20552-60. doi: 10.1021/ja208935u. Epub 2011 Nov 29.
Although the palladium-catalyzed Tsuji-Trost allylic substitution reaction has been intensively studied, there is a lack of general methods to employ simple benzylic nucleophiles. Such a method would facilitate access to "α-2-propenyl benzyl" motifs, which are common structural motifs in bioactive compounds and natural products. We report herein the palladium-catalyzed allylation reaction of toluene-derived pronucleophiles activated by tricarbonylchromium. A variety of cyclic and acyclic allylic electrophiles can be employed with in situ generated (η(6)-C(6)H(5)CHLiR)Cr(CO)(3) nucleophiles. Catalyst identification was performed by high throughput experimentation (HTE) and led to the Xantphos/palladium hit, which proved to be a general catalyst for this class of reactions. In addition to η(6)-toluene complexes, benzyl amine and ether derivatives (η(6)-C(6)H(5)CH(2)Z)Cr(CO)(3) (Z = NR(2), OR) are also viable pronucleophiles, allowing C-C bond-formation α to heteroatoms with excellent yields. Finally, a tandem allylic substitution/demetalation procedure is described that affords the corresponding metal-free allylic substitution products. This method will be a valuable complement to the existing arsenal of nucleophiles with applications in allylic substitution reactions.
虽然钯催化的 Tsuji-Trost 烯丙基取代反应已经得到了深入研究,但缺乏一般的方法来利用简单的苄基亲核试剂。这样的方法将有助于获得“α-2-丙烯基苄基”基序,这是生物活性化合物和天然产物中常见的结构基序。我们在此报告了钯催化的甲苯衍生的前亲核试剂的烯丙基化反应,该反应由三羰基铬活化。各种环状和非环状烯丙基亲电试剂可以与原位生成的(η(6)-C(6)H(5)CHLiR)Cr(CO)(3)亲核试剂反应。通过高通量实验(HTE)进行了催化剂鉴定,并得到了 Xantphos/钯的命中,这被证明是此类反应的通用催化剂。除了η(6)-甲苯络合物外,苄基胺和醚衍生物(η(6)-C(6)H(5)CH(2)Z)Cr(CO)(3)(Z = NR(2),OR)也是可行的前亲核试剂,允许与杂原子形成 C-C 键,产率优异。最后,描述了一种串联的烯丙基取代/脱金属反应程序,可得到相应的无金属烯丙基取代产物。该方法将是对现有亲核试剂库的有价值的补充,可应用于烯丙基取代反应。