FULL PAPER
DOI: 10.1002/ejic.200600407
First Example of a Gold(I) N-Heterocyclic-Carbene-Based Initiator for the
Bulk Ring-Opening Polymerization of L-Lactide
Lipika Ray,
[a]
Vimal Katiyar,
[a]
Mustafa J. Raihan,
[a]
Hemant Nanavati,
[a]
Mobin M. Shaikh,
[a]
and Prasenjit Ghosh*
[a]
Keywords: Carbenes / Functionalized NHC / Ring-opening polymerization (ROP) / Organometallic catalysis / Silver–NHC
complex / Gold–NHC complex
Synthesis, structure, and catalysis studies of two Au- and Ag-
based initiators, namely, [3-(N-tert-butylacetamido)-1-(2-hy-
droxycyclohexyl)imidazol-2-ylidene]AuCl (1c) and [3-(N-
tert-butylacetamido)-1-(2-hydroxycyclohexyl)imidazol-2-
ylidene]AgCl (1b), for the bulk ring-opening polymerization
of L-lactide are reported. Specifically, gold complex 1c was
obtained from silver complex 1b by the transmetalation reac-
tion with (SMe
2
)AuCl. Silver complex 1b was synthesized by
the treatment of 3-(N-tert-butylacetamido)-1-(2-hydroxycy-
clohexyl)imidazolium chloride (1a) with Ag
2
O. Compound 1a
was synthesized directly from the reaction of N-tert-butyl-
2-chloroacetamide, cyclohexene oxide, and imidazole. The
Introduction
The long-standing notion of gold being an expensive and
unreactive coinage metal with limited utility is gradually
changing. Various new applications of Au
I
complexes in
pharmaceuticals,
[1]
chemical vapor depositions,
[2]
and in
homogeneous catalysis
[3]
have been recently reported. Com-
pared to the other coinage metals (i.e. Cu and Ag), Au has
seen relatively few applications and poses a formidable chal-
lenge in utility-oriented research. Quite significantly, a re-
cent report detailed the use of a Au
I
complex supported
over a sterically demanding N-heterocyclic carbene (NHC)
ligand as a catalyst for the ethyl diazoacetate-assisted car-
bene-transfer reaction;
[3]
this represents an important
breakthrough in this field of chemistry and adds further
promise to the use of gold in chemical catalysis. The grow-
ing utility of NHCs in homogeneous catalysis is now well-
recognized, and a plethora of NHC-based catalysts have
been developed in recent years for a wide variety of trans-
formations, such as C–C coupling reactions,
[4,5]
olefin me-
tatheses,
[6]
hydrogenations,
[7,8]
hydroformylations,
[9]
hydro-
silylations,
[10]
CO-ethylene copolymerizations,
[11]
hydrobor-
ation
[12]
reactions, and so forth. Interestingly enough, de-
spite the numerous NHC-transition metal complexes that
[a] Department of Chemistry and Department of Chemical Engi-
neering, Indian Institute of Technology Bombay,
Powai, Mumbai 400 076, India
Fax: +91-22-2572-3480
E-mail: pghosh@chem.iitb.ac.in
© 2006 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim Eur. J. Inorg. Chem. 2006, 3724–3730 3724
molecular structures of 1a, 1b, and 1c have been determined
by X-ray diffraction studies. The formation of neutral mono-
meric complexes with linear geometries at the metal centers
was observed for both 1b and 1c. The Au and Ag complexes
1c and 1b successfully catalyzed the bulk ring-opening poly-
merization of L-lactide at elevated temperatures under sol-
vent-free melt conditions to produce moderate to low molec-
ular weight polylactide polymers with narrow molecular
weight distributions.
(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim,
Germany, 2006)
exist, the Au–NHC complexes are surprisingly few in
number and have seldomly been employed in catalysis.
[13]
A growing number of new applications have appeared
lately for the Ag
I
–NHC counterparts however, and their
catalytic utility has just begun to unfold.
[14,15]
Specifically,
the Ag
I
–NHC complexes have been found to be active cata-
lysts for several chemical transformations, such as, ethyl di-
azoacetate (EDA)-assisted carbene-transfer reactions,
[16]
catalytic preparation of 1,2-bis(boronate) esters,
[17]
transes-
terification reactions, and ring-opening lactide polymeriza-
tion reactions.
[18]
It is noteworthy that even though the ap-
plications of Ag
I
–NHC complexes in chemical catalysis is a
recent phenomenon, they are long-known for their use as
transmetalation agents for the synthesis of other transition
metal–NHC complexes.
[14,15]
Like its heavier congener, the
Au analogue, biomedical applications, particularly with re-
gard to antimicrobial activities, have recently been reported
for Ag
I
–NHC complexes.
[19,20]
Thus far, the popularity of
Ag–NHC complexes can be ascribed to their broadly based
applications, to their synthetic accessibility, and to their air
and moisture stabilities, which make them user-friendly and
hence convenient to handle.
[14,15]
As the catalytic utility of Au–NHC complexes remains
largely unexplored and that of the Ag–NHC complexes is
just beginning to emerge, we became interested in the design
of Au and Ag complexes for their potential application in
homogeneous catalysis. In particular, we were interested in