Complexation of a pyridyldiimine with iron(II) chloride; 2,6-bis[1-(2-isopropylphenylimino)ethyl]pyridine iron(II) chloride
SyntheticPage 437
DOI:
10.1039/SP437
Submitted Jul 06, 2010, published Jul 09, 2010
Chemicals Used
2,6-bis[1-(2-isopropylphenylimino)ethyl]pyridine page 436Fe4Cl8.THF6 (
doi:10.1016/S0020-1693(00)85366-9)
dichloromethane (Dried by heating to reflux for 72 h over CaH
2 then distilling)
diethyl ether (Dried by heating to reflux for 72 h over Na/K alloy then distilling, although other drying agents probably also adequate)
Procedure
2,6-bis[1-(2-isopropylphenylimino)ethyl]pyridine page 436 (0.50 g, 1.04 mmol) and Fe4Cl8.THF6 (0.24 g, 0.52 mmol, 0.5 eq.) were charged into a Schlenk vessel under argon. DCM (30 ml) was added and the reaction mixture was stirred at room temperature for 3 h, after which time the solution had become dark blue. The solution was filtered via cannula into a clean Schlenk vessel, and concentrated to ca 20 ml. Diethyl ether (60 ml) was added, and a blue precipitate formed. This was collected by filtration, washed with diethyl ether (20 ml) and dried in vacuo. (0.51 g, 82 %).
Author's Comments
This (and related) complexes are used as olefin polymerization catlaysts (see references).
Data
This complex is paramagnetic; however, a broad 1H NMR shows several assignable peaks. See lead reference for details.
Lead Reference
G. J. P. Britovsek, V. C. Gibson, S. K. Spitzmesser, K. P. Tellmann, A. J. P. White and D. J. Williams,
Dalton Trans., 2002, 1159
doi: doi: 10.1039/b106614p
Other References
G. J. P. Britovsek, V. C. Gibson, B. S. Kimberley, P. J. Maddox, S. J. McTavish, G. A. Solan, A. J. P. White and D. J. Williams, Chem. Commun., 1998, 849-850
doi:10.1039/a801933iB. L. Small, M. Brookhart and A. M. A. Bennett, J. Am. Chem. Soc., 1998, 120, 4049-4050
doi:10.1021/ja9802100
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Keywords: amines, heterocyclic compounds, Iron, organometallics, pyridyldiimine, substitution, transition metal catalysed
