Convenient One-Pot Synthesis of L2Pd(0) Complexes for Cross-Coupling Catalysis

Preston M. MacQueen, Ryan Holley, Subir Ghorai,Thomas J. Colacot

ORGANOMETALLICS(2023)

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摘要
A convenient one-pot synthesis of (tBu(3)P)(2)Pd(0) was successfully carried out by using various air-stable Pd(II) salts, such as Pd(cod)Cl-2, Pd(nbd)Cl-2, Pd(CH3CN)(2)Cl-2, or Pd(PhCN)(2)Cl-2, without the use of an external reducing agent. Using Pd(cod)Cl-2 as the precursor, large-scale synthesis of (tBu(3)P)(2)Pd(0) was accomplished in excellent yield and purity. Another protocol was also developed for L2Pd(0) complexes via an atom economical one-pot method by reacting in situ generated LPd(R-allyl)Cl complexes (L = tBu(3)P, Cy3P, (o-Tol)(3)P, CataXCium A, AmPhos, QPhos: R = H, Me, Ph) with 1 equivalent of L in the presence of a base with yields ranging from 74% to 92%, although the process can be further optimized. These methods are superior to those reported in the literature.
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