Amidation of zirconium tetrachloride with dimethylamidolithium; tetrakis(dimethylamido)zirconium
SyntheticPage 113
DOI:
10.1039/SP113
Submitted Aug 21, 2001, published Aug 21, 2001
Chemicals Used
toluene (distilled from sodium)
lithium dimethylamide (Aldrich) See also
synthesiszirconium 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