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Amide/halide metathesis at zirconium; bis(dimethylamido)bis(tetrahydrofuran)dichloro zirconium

SyntheticPage 401
DOI: 10.1039/SP401
Submitted Mar 09, 2010, published Mar 19, 2010
Peter Scott (peter.scott@warwick.ac.uk)
A contribution from Scott group, Warwick University


			Reaction Scheme: Amide/halide metathesis at <SPAN class=csm-chemical-name id=csm1283261799372 title=zirconium>zirconium</SPAN>

Chemicals Used

[Zr(NMe2)4synthesis
ZrCl4
diethyl ether
THF

Procedure

A Schlenk vessel with stirrer bar was charged with [Zr(NMe2)4] (synthesis) (0.49 g, 1.84 mmol) and zirconium tetrachloride (0.43 g, 1.85 mmol). To this was added diethyl ether (50 ml) followed by THF (10 ml). The solution was stirred for 2 h during which time it turned a pale green colour. The solution was stirred for a further 2 h, filtered and concentrated. Upon keeping at –30 ºC for 48 h, a yellow/green crystalline solid had formed. This was filtered, washed with pentane at –78 ºC and dried in vacuo. Yield = 1.01 g, 70 %

Author's Comments

It is sometimes noted that a fine solid remains undissolved, but upon gentle warming all solids dissolved. It's important to do this otherwise the product is contaminated with ZrCl4. See here for comments on purity of ZrCl4.

Data

1H NMR 300 MHz (d6-benzene) δ ppm 3.70 (m, 8H, THF), 3.31 (s, 12H, NMe2), 1.08 (m, 8H, THF).

Lead Reference

Brenner, S.; Kempe, R.; Arndt, P. Z. Anorg. Allg. Chem., 1995, 621, 2021 doi:10.1002/zaac.19956211207

Other References

For a use of this compound in synthesis see:
Paul D. Knight, Ian J Munslow, Paul N. O'Shaughnessy and Peter Scott, Chem. Commun., 2004, 894 - 895 doi:10.1039/b401493f

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Keywords: metathesis, organometallics, zirconium Zr chloride dimethylamido dimethylamide

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