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Amidation of zirconium tetrachloride with dimethylamidolithium; tetrakis(dimethylamido)zirconium

SyntheticPage 113
DOI: 10.1039/SP113
Submitted Aug 21, 2001, published Aug 21, 2001
Colin Morton (c.morton@warwick.ac.uk)
A contribution from Scott group, Warwick University
Reaction Scheme: Amidation of zirconium tetrachloride with dimethylamidolithium

Chemicals Used

toluene (distilled from sodium)
lithium dimethylamide (Aldrich) See also synthesis
zirconium tetrachloride (Aldrich)

Procedure

Toluene (80 ml) was added to a mixture of [Li(NMe2)] (3.7 g, 0.068 mol) and ZrCl4 (4.0 g, 0.017 mol) at room temperature. After stirring overnight, the solvent was removed in vacuo and the yellow residue was sublimed at 80°C and 10-3 mbar giving an off-white crystalline solid. Yield = 83%, 3.7g.

Author's Comments

Standard schlenk line procedures are used. The sublimation was carried out using schlenk-line vacuum. We have carried out this procedure many times.

Data

1H NMR (293 K, d6-benzene) 3.05 (s, 24H, NMe2).

Lead Reference

D. C. Bradley and I. M. Thomas, J. Chem. Soc., 1960, 3857.

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Keywords: 113, amido, organometallic starting materials, zirconium