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Fig. 2.16
Synthesis and complexation of the bis(phosphine)s
13x
.
12b-d
were treated with an equimolar amount of
n
-butyllithium at -70
C in dry
tetrahydrofuran. Subsequently, 1,2-bis(dichlorophosphino)ethane was introduced.
After work-up, pure 1,2-bis(di(2,4,6-trimethylphenyl)phosphino)ethane (
13b
), 1,2-
bis(di(2-isopropylphenyl)phosphino)ethane (
13 c
) and 1,2-bis(di(2,4,6-triisopropyl-
phenyl)phosphino)ethane (
13d
) were obtained in moderate to high yields after re-
crystallization of the crude product (Fig. 2.16). Yields of more than 90% for
13b
compared to 19% obtained using the method of Chatt et al. [53] clearly underline
the big advantage of this straightforward procedure.
The reaction of
13x
with bis(benzonitrile)dichloropalladium(II) [Bn
2
PdCl
2
] and
monochloro(1,5-cyclooctadiene)monomethylpalladium(II) [(COD)PdClMe] yielded
the corresponding palladium(II) complexes
14x
and
15 x
(Fig. 2.16). Upon slow
evaporation of an acetonitrile solution,
14c
and
14d
gave crystals that were suit-
able for structure determination via single crystal X-ray diffraction (Fig. 2.17).
Compound
14b
was crystallized by slow diffusion of pentane into a solution of
14b
in tetrachloroethane.
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