催化 Pd 的氧化联合反应在芳香的 CH 激活和新公司和 CC 契约的形成是很重要的。Sanford 开创了采用 Pd (OAc ) 的实际、指导 CH 激活反应 2 作为催化剂自从 2004。然而直到现在,推测的反应 Pd (IV ) 在这些反应的短暂中介没从反应被孤立或直接检测了答案。Electrospray 电离双人脚踏车团 spectrometry (ESI-MS/MS ) 被用来拦截并且描绘反应 Pd (IV ) 在 Pd (OAc ) 2-catalyzed 的答案的短暂中介氧化联合反应。在这研究, Pd (IV ) 短暂中介从 Pd (OAc ) 2-catalyzed 的答案被检测由 ESIMS 和在反应系统的短暂中介是的拦截 Pd (IV ) 的 MS/MS 的氧化联合反应有综合真 Pd (IV ) 建筑群的一样。我们的 ESIMS (/MS ) 研究证实了 Pd (IV ) 反应的存在短暂中介。最有趣地,短暂中介显示出的 Pd (IV ) 的 MS/MS 减少的消除反应到有进在煤气的阶段的产品的新公司契约形成的 Pd (II ) 建筑群在答案的短暂中介。
Pd-catalyzed oxidative coupling reaction was of great importance in the aromatic C--H activation and the for-mation of new C-O and C--C bonds. Sanford has pioneered practical, directed C-H activation reactions em-ploying Pd(OAc)2 as catalyst since 2004. However, until now, the speculated reactive Pd(Ⅳ) transient intermedi-ates in these reactions have not been isolated or directly detected from reaction solution. Electrospray ionization tandem mass spectrometry (ESI-MS/MS) was used to intercept and characterize the reactive Pd(Ⅳ) transient inter-mediates in the solutions of Pd(OAc)2-catalyzed oxidative coupling reactions. In this study, the Pd(IV) transient in-termediates were detected from the solution of Pd(OAc)2-catalyzed oxidative coupling reactions by ESI-MS and the MS/MS of the intercepted Pd(IV) transient intermediate in reaction system was the same with the synthesized au-thentic Pd(Ⅳ) complex. Our ESI-MS(/MS) studies confirmed the presence of Pd(Ⅳ) reaction transient intermedi-ates. Most interestingly, the MS/MS of Pd(Ⅳ) transient intermediates showed the reductive elimination reactivity to Pd(Ⅱ) complexes with new C-O bond formation into product in gas phase, which was consistent with the proposed reactivity of the Pd(Ⅳ) transient intermediates in solution.