Ferocenne

             All reagents were provided by the Chemistry 108 laboratory and used without additional purification. All solvents were removed by rotary evaporation. All reaction products were isolated with vacuum filtration, unless otherwise stated. Infrared spectra were recorded on a Perkins-Elmer 1600 series FTIR Spectrometer using Nujol mulls and KBr pellets. 1H and 13C nuclear magnetic spectra were taken in CDCl3 at 300 MHz on an AMX Spectrometer. Ultra-violet-visible spectroscopy was performed using quartz cuvettes on a Hewlett-Packard 8452A Diode Array Spectrometer. All thin layer chromatography was performed in a solvent system.
             In a 100mL round-bottom flask iron (II) chloride tetrahydrate (5g, mmol) was dissolved in nitrogen degassed DMSO (30mL) and stirred for 1h. The solution was stoppered to prevent oxidation. Diethyl ether (80mL) and flake KOH (20g, mmol) was added to a 500mL three-neck flask equipped with an egg-shaped stir bar, a stopper in the central neck, a 100mL addition funnel fitted with a side arm adapter (connected to a nitrogen source) in one neck, and a condenser in the other neck. The mixture was flushed with nitrogen and then stirred vigorously. Under a nitrogen-counter flow cyclopentadiene (4.25mL) was added to the mixture. Nitrogen flow was discontinued after ca. 15 minutes and the iron (II) chloride solution was added dropwise via the addition funnel and the mixture was stirred for 30 minutes. Additional diethyl ether (ca. 20mL) was added to make the ethereal layer easier to decant. The organic layer was washed with 2M HCl (2 X 20mL) to neutralize the alkali and water (2 X!
             20mL). The organic layer was poured into an evaporating dish and the ether was allowed to evaporate. After evaporation 0.59 g of orange crystals were afforded (%). A small sample of ferrocene was purified by sublimation. A 1H
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Ferocenne . (1969, December 31). In MegaEssays.com. Retrieved 19:24, April 25, 2024, from https://www.megaessays.com/viewpaper/66960.html