Angewandte
Chemie
DOI: 10.1002/anie.201403410
Homogeneous Catalysis
Palladium-Catalyzed Allylic Alkylation of Simple Ketones with Allylic
Alcohols and Its Mechanistic Study**
Xiaohong Huo, Guoqiang Yang, Delong Liu, Yangang Liu, Ilya D. Gridnev,* and
Wanbin Zhang*
Abstract: Allylic alcohols were directly used in Pd-catalyzed
allylic alkylations of simple ketones under mild reaction
conditions. The reaction proceeded smoothly at 208C by the
concerted action of a Pd catalyst, a pyrrolidine co-catalyst, and
a hydrogen-bonding solvent, and does not require any addi-
tional reagents. A computational study suggested that methanol
plays a crucial role in the formation of the p-allylpalladium
complex by lowering the activation barrier.
Therefore, a simple and convenient method for the direct
use of allylic alcohols is highly desired.
We have demonstrated that allylic amines and allylic alkyl
ethers possessing challenging leaving groups have been
successfully utilized to form p-allylpalladium complexes
through hydrogen-bond activation (Scheme 1).[9] Just before
T
he palladium-catalyzed allylic alkylation is a powerful
À
synthetic tool for C C bond formation and has a broad range
of applications in the synthesis of biologically important
molecules.[1,2] One of the general features of this transforma-
tion is that substrates with a wide range of activated leaving
groups (acetates, carbonates, etc.) can be utilized to form p-
allylpalladium complexes.[3] However, the direct use of the
accessible allylic alcohols in Pd-catalyzed allylic alkylations
remains a challenge. It is worth noting that the use of allylic
alcohols as substrates would help to avoid the additional steps
required for the preparation of the corresponding activated
substrates and the formation of at least stoichiometric
amounts of waste both in the preparation and substitution
steps. Therefore, allylic alcohols are gaining increasing
attention as ideal substrates for palladium-catalyzed allylic
alkylation reactions[4–7] with regard to waste minimization and
sustainability.[8] While there have been some reports of Pd-
catalyzed allylic alkylations using allylic alcohols, most of
these methods required activators[4,6] or special ligands.[7]
Scheme 1. Reactions of allylic substrates with challenging leaving
groups. Bn=benzyl, Cy=cyclohexyl, dppf=1,1’-bis(diphenylphospha-
nyl)ferrocene, Nu=nucleophile.
the submission of this manuscript, Ohshima and co-workers
reported an interesting platinum- and pyrrolidine-catalyzed
direct allylic alkylation of b-keto carbonyl compounds
with allylic alcohols using acetic acid as an additive under
high temperature and microwave conditions.[5h,10] We herein
report a simple method for the direct use of allylic alcohols in
Pd-catalyzed allylic alkylations of simple ketones in the
presence of a pyrrolidine co-catalyst in alcohol solvents under
mild conditions, and a mechanistic study of this reaction
(Scheme 1).
[*] X. Huo, Prof. D. Liu, Prof. Y. Liu, Prof. W. Zhang
School of Pharmacy, Shanghai Jiao Tong University
800 Dongchuan Road, Shanghai 200240 (China)
E-mail: wanbin@sjtu.edu.cn
Dr. G. Yang, Prof. W. Zhang
School of Chemistry and Chemical Engineering
Shanghai Jiao Tong University (China)
Initially, we investigated the Pd-catalyzed allylic alkyla-
tion of cyclohexanone with cinnamyl alcohol in several
solvents, using a [Pd(h3-C3H5)Cl]2/dppf catalyst system and
1.0 equivalent of pyrrolidine at 208C.[11] We found that the
reaction proceeded well in alcohol solvents and that methanol
showed the most promising results. The reaction temperature
and the amounts of cyclohexanone and pyrrolidine were also
screened and the optimal reaction conditions were: cinnamyl
alcohol/ketone = 1.1:1, 20 mol% pyrrolidine, and 2.5 mol%
[Pd(h3-allyl)Cl]2/dppf as a catalyst in methanol at 208C. The
effect of an acid as a co-catalyst was also explored, as it can
catalyze both the formation of the enamine and the ionization
of the leaving group.[5h,6b–d] The results suggested that our
Prof. I. D. Gridnev
Department of Chemistry, Graduate School of Science
Tohoku University
Aramaki 3-6, Aoba-ku, Sendai 9808578 (Japan)
E-mail: igridnev@m.tohoku.ac.jp
[**] Computational results in this research were obtained using super-
computing resources at the Information Synergy Center, Tokyo
Institute of Technology. This work was partially supported by the
National Natural Science Foundation of China (No. 21172143,
21172145, 21372152, and 21232004), the Nippon Chemical Indus-
trial Co., Ltd, Shanghai Jiao Tong University, and the CAMPUS Asia
Program of Tohoku University.
Supporting information for this article is available on the WWW
Angew. Chem. Int. Ed. 2014, 53, 1 – 6
ꢀ 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
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