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

被引:6
作者
MacQueen, Preston M. [1 ]
Holley, Ryan [1 ]
Ghorai, Subir [1 ]
Colacot, Thomas J. [1 ]
机构
[1] MilliporeSigma, Life Sci Chem, Res & Dev, Milwaukee, WI 53209 USA
关键词
FACILE INTRAMOLECULAR METALATION; TRI-TERT-BUTYLPHOSPHINE; REDUCTION-MECHANISM; OXIDATIVE ADDITION; HIGHLY EFFICIENT; PALLADIUM(II); PD(II); ARYL; ARYLATION; PRECURSOR;
D O I
10.1021/acs.organomet.3c00059
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
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.
引用
收藏
页码:2644 / 2650
页数:7
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