Current Green Chemistry
Mukund Ghavre
a,b,d,*
, Brid Quilty
c
and Nicholas Gathergood
b,e,*
a
School of Chemical Sciences and National Institute of Cellular Biotechnology, Dublin City University, Glasnevin, Dub-
lin 9, Ireland;
b
SFI SRC in Solar Energy Conversion, UCD School of Chemical & Bioprocess Engineering, Engineering
& Materials Science Centre, UCD Dublin, Belfield, Dublin 4, Ireland;
c
School of Biotechnology, Dublin City University,
Glasnevin, Dublin 9, Ireland;
d
Department of Chemistry, Brock University, 1812 Sir Isaac Brock Way, St. Catharines,
L2S 3A1 ON, Canada;
e
Department of Chemistry, Chair of Green Chemistry, Tallinn University of Technology, Aka-
deemia tee 15, Tallinn, Estonia
A R T I C L E H I S T O R Y
Received: August 11, 2015
Revised: June 14, 2016
Accepted: June 15, 2016
DOI:
10.2174/221334610366616072811
5628
Abstract: Background: Low toxicity ionic liquids (ILs) have shown a wide range of
applications in material chemistry, synthetic chemistry, and green chemistry. They
can be considered as 'green' alternatives to the conventional solvents, as their unique
properties can offer additional benefits. In our previous reports, we have shown that
such ILs can be used as reaction media in hydrogenation, carbonyl-ene reactions, and
Brønsted acid catalyzed reactions.
Methods: Low toxicity ILs are prepared by a short synthesis. The palladium based
catalyst bearing an asymmetric ligand is immobilized in these ILs. This ‘green’ cata-
lytic system is employed for enantioselective Tsuji-Trost reactions. For comparison,
several reactions are run in conventional solvents.
Results: The reactions in ILs provide good to excellent enantiomeric excess, however, low yields are
obtained compared to the conventional solvents. The catalytic system is recyclable.
Conclusion: Conventional solvent (DMSO) is proved to be superior to our ILs, however, the results in
our ILs are an improvement over [bmim] ILs. The low yields are attributed to high viscosity of the ILs,
and we propose can be resolved by tuning the viscosity of the IL by anion exchange.
Keywords: Enantioselectivity, ionic liquids, Pd-catalysis, recyclable, Tsuji-Trost reaction.
1. INTRODUCTION
The Tsuji-Trost reaction is one of the classical coupling
methods to form C-C bonds using transition metal catalysts.
A unique feature of this reaction is replacement of a leaving
group on an allylic carbon with a range of suitable nucleo-
philes. The Tsuji-Trost reaction is an important methodology
in the preparation of allyl substituted organic molecules [1].
Asymmetric Tsuji-Trost reactions have been developed for
the synthesis of enantiopure drug molecules [2].
Ionic liquids (ILs) have been investigated as reaction
media in transition metal catalysis for over a decade. This is
mainly because of their properties, such as low vapor pres-
sure [3], non-flammability, high boiling point, and high di-
electric constant. There are many examples demonstrating
the use of ILs in hydrogenation [4], Heck [5], Suzuki [6],
carbonyl-ene [7] and Diels-Alder reactions [8]. A number of
investigations have been made to apply ILs in Tsuji-Trost
*Address correspondence to these authors at the Department of Chemistry,
Chair of Green Chemistry, Tallinn University of Technology, Akadeemia
tee 15, Tallinn, Estonia; Tel: +372-620-4381;
E-mail: Nicholas.Gathergood@ttu.ee; and Department of Chemistry, Brock
University, 1812 Sir Isaac Brock Way, St. Catharines, L2S 3A1 ON,
Canada; Tel: 905-688-5550 (4174); E-mail: mghavre2@brocku.ca
reactions [9-15] as well as reactions with chitosan supported
catalysts [16], microwave assisted reactions [17], and reac-
tions in ILs-organic solvent biphasic media [18]. Toma et al.
[19, 20] reported enantioselective Tsuji-Trost reactions in
[bmim][PF
6
] (1-butyl-3-methyl-imidazolium hexafluoro-
phosphate) using a range of homochiral ferrocenyl phosphine
ligands.
ILs, may be considered 'green' alternatives to conven-
tional solvents and can offer a number of benefits in chemi-
cal processes. They can solubilize a wide range of inorganic
and organic compounds, including immobilizing reagents
and catalysts in one phase. ILs can also be utilized in high
vacuum systems due to low vapor pressure, and can be recy-
clable [21]. Additionally, low toxicity and biodegradable ILs
have potential to be less harmful to ecosystem than the con-
ventional solvents [22]. Reported data on the toxicity of
[bmim] based ILs show that some examples are less toxic
than conventional solvents [e.g. toluene, acetonitrile, DCM
(dichloromethane) and DMSO (dimethyl sulfoxide)] [23].
The toxicity of [Rmim] (1-alkyl-3-methylimidazolium) ILs
with a long hydrocarbon side chain (R = C
6
-C
10
) have been
determined to exhibit higher antimicrobial activity than
shorter alkyl groups (e.g. R = C
1
-C
4
) [24]. Hence, we chose
to incorporate heteroatoms into the alkyl side chains, predict-
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Current Green Chemistry, 2016, 3, 181-189
181
RESEARCH ARTICLE
Enantioselective Tsuji-Trost Reactions in Low Toxicity Ionic Liquids