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Continuous extraction of iron(II) chloride into THF; Fe4Cl8(THF)6

SyntheticPage 456
DOI: 10.1039/SP456
Submitted Aug 02, 2010, published Aug 25, 2010
lihong li (lihong.li@warwick.ac.uk)
A contribution from Scott group, Warwick University


			Reaction Scheme: Continuous extraction of <SPAN class=csm-chemical-name id=csm1282745570858 title="iron(II) chloride">iron(II) chloride</SPAN> into <SPAN class=csm-chemical-name id=csm1282745550848 title=THF>THF</SPAN>

Chemicals Used

FeCl2 (STREM)
THF

Procedure

A dry glass fibre Soxhlet thimble was charged with anhydrous iron(II) chloride (5.0 g, 39.4 mmol) inside an inert gas glove box and connected to a round-bottomed Schlenk flask filled with anhydrous THF (200 cm3). The apparatus was purged thoroughly with argon and the solvent heated under reflux for 4 d by which time all the metal chloride had been extracted. The compound had already begun to separate as a white microcrystalline solid. The solution was left to cool to ambient temperature and concentrated to ca. 50cm3 before the solid was collected by cannula filtration and dried in vacuo for 3 h. (8.5 g, 92 %).

Author's Comments

Procedure hads been carried out many times by several members of the group.

Data

Anal. Found (Calcd. For C12H24Cl4Fe2O3): C 30.58 (30.68); H 5.16 (5.15) %


Lead Reference

Adapted from F. A. Cotton, R. L. Luck and K. A. Son, Inorg. Chim. Acta, 1991, 179, 11
doi:10.1016/S0020-1693(00)85366-9 where the compound is prepared from FeCl3 and Fe in THF. See also G. Wilkinson, Org. Synth., 1956, 36, 31.

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