Addition of THF to iron(II) chloride via Sohxlet extraction; Fe4Cl8.6THF
SyntheticPage 642
DOI:
10.1039/SP642
Submitted Jul 22, 2013, published Jul 25, 2013
Chemicals Used
Anhydrous iron(II) chloride (STREM Chemicals)
THF (distilled over potassium)
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 fitted to the Soxhlet extractor. The upper and lower joints were sealed with cones, caps or Suba Seals as appropriate. Outside the box a round-bottomed, side-arm Schlenk flask filled with anhydrous THF (200 cm3) and an efficient condenser with gas bubbler were fitted. The apparatus was purged thoroughly with argon (or dinitrogen) and the solvent was heated so as to effect gentle extraction for 4 d. By this 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 was carried out under argon by using a glovebox and dual manifold vacuum/argon line and standard Schlenk techniques. Ensure that you are not heating a closed system. We use a T-piece connector at the top of the condenser with a gentle gas flow to a bubbler, or sometimes a one-piece inert gas bubbler.
Data
Anal. Found (Calcd. For C12H24Cl4Fe2O3): C 30.58 (30.68); H 5.16 (5.15) %.
Lead Reference
Cotton, F. A., Luck, R. L. and Son, K. A.,
Inorg. Chim. Acta., 1991,
179, 11
http://dx.doi.org/10.1016/S0020-1693(00)85366-9,
Other References
Sella's Classic Kit article on Soxhlet,
Chemistry World,Sept. 2007
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Keywords: addition, inorganic compounds, iron chloride, Tetrahydrofuran