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Addition of tetrahydrofuran to titanium tetrachloride; Tetrachlorobis(tetrahydrofurn)titanium(IV)

SyntheticPage 617
DOI: 10.1039/SP617
Submitted Jul 11, 2013, published Jul 15, 2013
Max Hammond (max@flipstorm.net), Pratik Gurnani (pratik.gurnani@warwick.ac.uk)
A contribution from Scott group, Warwick University


			Reaction Scheme: <IMG src="/images/empty.gif">Addition of <SPAN id=csm1374251075218 class=csm-chemical-name title=tetrahydrofuran grpid="2">tetrahydrofuran</SPAN> to <SPAN id=csm1374251120954 class=csm-chemical-name title="titanium tetrachloride" grpid="4">titanium tetrachloride</SPAN><IMG src="/images/empty.gif">

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

None taken

Lead Reference

L. E. Manzer, Inorganic Syntheses, 1982, 21, 135-140. http://dx.doi.org/10.1002/9780470132524.ch31

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Keywords: addition, inorganic compounds, tetrahydrofuran, titanium tetrachloride