1) Complexation of a pyridyldiimine with iron(II) chloride

SyntheticPage 437
Published Jul 09, 2010


Reaction Scheme

Procedure

2,6-bis[1-(2-isopropylphenylimino)ethyl]pyridine page 436 (0.50 g, 1.04 mmol) and Fe4Cl8.THF6 (0.24 g, 0.52 mmol, 0.5 eq.) were charged into a Schlenk vessel under argon. DCM (30 ml) was added and the reaction mixture was stirred at room temperature for 3 h, after which time the solution had become dark blue. The solution was filtered via cannula into a clean Schlenk vessel, and concentrated to ca 20 ml. Diethyl ether (60 ml) was added, and a blue precipitate formed. This was collected by filtration, washed with diethyl ether (20 ml) and dried in vacuo. (0.51 g, 82 %).

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2) Continuous extraction of iron(II) chloride into THF

SyntheticPage 456
Published Aug 25, 2010


Reaction Scheme

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 %).

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3) Addition of THF to iron(II) chloride via Sohxlet extraction

SyntheticPage 642
Published Jul 25, 2013


Reaction Scheme

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 %).

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