Addition of tetrahydrofuran to titanium tetrachloride; Tetrachlorobis(tetrahydrofurn)titanium(IV)
SyntheticPage 617
DOI:
10.1039/SP617
Submitted Jul 11, 2013, published Jul 15, 2013
Chemicals Used
Titanium tetrachloride (Aldrich)
Dichloromethane (distilled over calcium hydride)
THF (distilled over potassium)
Procedure
A Schlenk vessel with stirrer bar was charged with dichloromethane (30 ml) and titanium tetrachloride (2.9 ml, 26.4 mmol). The solution was stirred vigorously and THF (9 ml, 111.1 mmol) was added dropwise over 1 h. The solution was stirred for a further 20 m. Pentane (60 ml) was added, and then the solution was cooled to –30 ºC and kept overnight to yield a bright yellow crystalline solid. This was recovered by filtration and dried in vacuo, yielding [TiCl4(THF)2] (8.1 g, 92 %).
Author's Comments
Procedure was carried out under an atmosphere of argon using a dual-manifold vacuum/argon line and standard Schlenk procedures,
Data
Lead Reference
L. E. Manzer,
Inorganic Syntheses, 1982,
21, 135-140.
http://dx.doi.org/10.1002/9780470132524.ch31
This page has been viewed approximately 6591 times since records began.
Get structure file (.cdx, .sk2, .mol)
Keywords: addition, inorganic compounds, tetrahydrofuran, titanium tetrachloride