33
Full Paper
Macromolecular
Chemistry and Physics
wileyonlinelibrary.com DOI: 10.1002/macp.201200544
Reactivity of the Dicationic Ruthenium–
Alkylidene Complex [Ru(DMF)
3
(IMesH
2
)(=CH—
2—(2—PrO)—C
6
H
4
)],
2 +
(BF
4
-
)
2
] in Ring-Opening
Metathesis and Cyclopolymerization
Benjamin Autenrieth, Emily Baird Anderson, Dongren Wang,
Michael R. Buchmeiser*
The reactivity of the dicationic Ru–alkylidene complex [Ru(DMF)
3
(IMesH
2
)(—CH—2—(2—
PrO)—C
6
H
4
)]
2 +
(BF
4
-
)
2
] ( 1, IMesH
2
= 1,3-dimesitylimidazolin-2-ylidene) in the ring-opening
metathesis polymerization (ROMP) of various functional norborn-2-enes as well as in the
cyclopolymerization of different 1,6-heptadiynes is reported. Due to its dicationic character,
complex 1 is highly electrophilic and possesses high reactivity towards alkenes and 1,6-hep-
tadiynes. Generally, a pronounced difference in reactivity between monomers bearing coordi-
nating groups and those that lack such moieties is observed.
In the presence of ionic monomers containing coordinating
anions such as Br
-
and I
-
, a rapid change in the nature of the
propagating alkylidene from a dicationic to a neutral one is
observed.
B. Autenrieth, E. B. Anderson, D. Wang, M. R. Buchmeiser
Lehrstuhl für Makromolekulare Stoffe und Faserchemie,
Institut für Polymerchemie, Universität Stuttgart,
Pfaffenwaldring 55, 70569 Stuttgart, Germany
E-mail: michael.buchmeiser@ipoc.uni-stuttgart.de
M. R. Buchmeiser
Institut für Textilchemie und Chemiefasern Denkendorf,
Körschtalstr. 26, 73770 Denkendorf, Germany
centers out of a second, nonpolar, liquid transport phase.
In 1, the Ru=C double bond is strongly polarized com-
pared with neutral Ru–alkylidene complexes. Evidence for
polarization is the observed shift of the alkylidene-signal
in the
1
H NMR spectrum from δ = 16.58 ppm (CD
2
Cl
2
) for
the parent second-generation Grubbs-Hoveyda initiator
to δ = 19.28 ppm (CD
2
Cl
2
) in 1, also indicating a strong
agostic interaction between the alkylidene-proton and
the ruthenium. Such pronounced downfield shifts in the
1
H NMR for the alkylidene proton are also observed for
several “pseudohalide”-derivatives of Grubbs- or Grubbs-
Hoveyda-type initiators (Table S1, Supporting Informa-
tion)
[2–8]
where a strong polarization of the Ru–alkylidene
has been suggested by DFT calculations.
[9]
Here, we report on the reactivity of 1, which in fact is a
rare example of dicationic Ru–alkylidenes, in ring-opening
metathesis polymerization (ROMP). However, in view of
the strong propensity of the above-mentioned pseudo-
halide derivatives of Grubbs- and Grubbs-Hoveyda-type
initiators to cyclopolymerize 1,6-heptadiynes, we were
1. Introduction
We recently reported on the synthesis of the dicationic
Ru–alkylidene complex [Ru(DMF)
3
(IMesH
2
)(=CH—2—(2—
PrO)—C
6
H
4
)]
2 +
(BF
4
-
)
2
] ( 1, IMesH
2
= 1,3-dimesityl-imida-
zolin-2-ylidene, Figure 1) and its use in cross-metathesis
reactions in ionic liquids under continuous biphasic liquid/
liquid conditions.
[1]
Due to its dicationic character, 1 can be
immobilized within a polar liquid phase, for example, an
ionic liquid, whereas the reactants diffuse to the catalytic
Macromol. Chem. Phys. 2013, 214, 33−40
© 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim