evil_lurker
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Registered: 12-3-2005
Location: United States of Elbonia
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Mood: On the wagon again.
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Iron pentacarbonyl synthesis...
I can't seem to find any sort of information on how this compound is produced... I've googled the hell out of it and dug thru a crapload of patents,
but none deal with the actual synthesis.
I'm thinking that maybe using a flask with some activated iron powder, evacuate with a vacuum pump, then pressurize with carbon monoxide @60-100ºC
and leave sitting in the dark for a couple days and see what happens.
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matei
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Registered: 16-9-2006
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Check Brauer - "Inorganic Synthesis".
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benzylchloride1
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Registered: 16-3-2007
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I am currently researching methods of producing this compound at atmospheric pressure. I found a procedure that looks to be fairly simple for
producing this compound in small amounts from fairly easy to obtain chemicals. Here is the procedure from Synthesis of Organometallic Compounds:
Iron powder (5.0 g) is suspended in dry heptane (30 mL) and is activated by shaking
for 15 min in an atmosphere of H 2 S, A slight gas evolution on the surface of the iron
particles is observed during the activation. The suspension is then stored under nitro-
gen. After introduction of DCO or C I8 0 at atmospheric pressure, the suspension is
stirred at room temperature very vigorously for 20 h. The solution gradually turns red
during the reaction. The solvent is then removed under reduced pressure. The title
product is obtained by distillation at atmospheric pressure (bp 103 0q.
Properties: mp -20°C. bp 103°C. IR [Fe(CO)s in C 6 H I2 ]: 2022, 2000 cm- I .
[Fe(COkl 3 CO)n]: 2023, 200 I, 1988, 1976, 1972, 1964, 1955 cm- l ; [Fe(COkn(C I8 0)n]:
2023,2008,200 I, 1988, 1976, 1964, 1955 cm I.
Pentacarbonyliron is a straw-colored liquid with a musty odor, which is stable in air
at room temperature. It should be handled in a hood because it is a toxic liquid with a
relatively high vapor pressure even at room temperature (21 mmHg, 20°C). It should
be stored in the dark to prevent slow decomposition.
The iron powder can be obtained from hand warmers. Certain disposable hand warms have finely divided iron in them that rapidly reacts with oxygen for
produce heat and iron oxide. The hand warmer would have to be opened up under the heptane due to the air sensitive nature of the finely divided iron.
The carbon monoxide could be produced by reacting oxalic or formic acid with concnetrated sulfuric acid. Be sure to conduct this step in a powerful
exhaust hood or out side on a breezy day due to the highly poisonous nature of the carbon monoxide and the pentacarbonyl iron product. I have not
conducted this procedure, but I plan on running it in the near future.
[Edited on 11-1-2009 by benzylchloride1]
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