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Titanium(0) Arene Complexes: Synthesis and X-ray Crystal Structure of [η6-C10H8Ti{tBuSi(CH2PMe2)3}]

✍ Scribed by Thomas G. Gardner; Prof. Dr. Gregory S. Girolami

Publisher
John Wiley and Sons
Year
1988
Tongue
English
Weight
520 KB
Volume
27
Category
Article
ISSN
0044-8249

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✦ Synopsis

To a stirred solution of [TiC13(trimpsi)(thf)] (3.90 g, 7.27 mmol) in tetrahydrofuran (50 mL) at -78°C was added naphthalenesodium (150 mL, 0.145 M in THF, 21.8 mmol). A red-purple solution formed immediately. The solution was warmed to room temperature slowly, and the solvent was removed in vacuum. The excess naphthalene was removed by sublimation in vacuum at 25°C. The dark purple residue was extracted with diethyl ether (5 x 200 mL), and the combined extracts were concentrated to 200mL and cooled to -20°C to give dark purple crystals of 1. Yield: 1.4 g (40%); m.p. 196-204°C. Correct elemental analysis (C,H,Ti).

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