Aqua-regia
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Dicyanobis(1,10-phenanthrolin)Fe(II)
How would prepare this compound from common reagents? I didn't find anything about this stuff. (Alfa Ventron 12 189)
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UnintentionalChaos
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You'd need to prepare 1,10-phenanthroline. The easiest way to do this is probably via the skraup quinoline synthesis using o-phenylenediamine instead
of aniline.
Knowing that the abbreviation "phen" is often used instead of 1,10-phenanthroline when discussiing it's complexes may help your search.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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Klute
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Have you checked Inorganic Synthesis? I'lll have a look if you want monday at work..
\"You can battle with a demon, you can embrace a demon; what the hell can you do with a fucking spiritual computer?\"
-Alice Parr
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Aqua-regia
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I've preparated the1,10-phenanthroline yet. It was a nasty work. (Unendless extraktion with benzene, see Vogel) The next step, what I need, building
the above complex. Probably 1,10-phenanthroline with FeSO4 or Fe(II)NH4)2 SO4 to bring to boil in water, then add KCN. Precipitate? I will try it.
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Aqua-regia
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Not yet, i'll to look it first on Monday too.
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Polverone
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It's in Inorganic Syntheses Volume 12.
| Quote: | This synthesis should be performed in the hood. Potassium cyanide hydrolyzes under appropriate conditions to generate hydrogen cyanide.
The dark-red solution obtained on dissolving 6.0 g. (0.030 mole) of 1,10-phenanthroline monohydrate together with 3.9 g. (0.010 mole) of ferrous
ammonium sulfate hexahydrate in 400 ml. of water is heated to just below the boiling point. A freshly prepared solution of 10 g. of potassium cyanide
in 20 ml. of
water is added all at once to the hot solution. After thorough stirring, the hot mixture is set aside to cool at room temperature. Dark violet, almost
black, dense, fine crystals develop rapidly. Precipitation is complete within several minutes; however, an aging period of an hour or longer is
considered beneficial. The yield of crude product, after filtration and generous washing with water, is approximately 5 g. The filtrate contains about
2 g. of free 1,10-phenanthroline that can be recovered by extraction with either benzene or diethyl ether.
For purification, the crude product is dissolved in 30 ml. of concentrated sulfuric acid. To the vigorously stirred solution 1 l. of water is slowly
added. The recrystallized product is collected by suction filtration and washed thoroughly with small portions of water until free of sulfuric acid. A
final rinse with acetone facilitates drying. The product is vacuum-dried at room temperature. The final yield ranges from 4.0 to 4.9 g. (80-98% based
on the iron(II) salt). |
PGP Key and corresponding e-mail address
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Aqua-regia
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Thanks Polverone!
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JohnWW
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A closely related compound, o-phenanthroline, is a standard colorimetric and spectrophotometric reagent for testing for iron in waters. It produces an
intense red color with traces of dissolved Fe.
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UnintentionalChaos
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Quote: Originally posted by JohnWW  | | A closely related compound, o-phenanthroline, is a standard colorimetric and spectrophotometric reagent for testing for iron in waters. It produces an
intense red color with traces of dissolved Fe. |
o-phenanthroline is 1,10-phenanthroline.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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benzylchloride1
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Aqua Regia, how did you prepare the 1,10-phenanthroline. Did you use arsenic acid as the directions in Vogel specify. I am interested in
1,10-phenanthroline, but I do not have arsenic acid available. I am looking for another method of running this synthesis without using arsenic. The
normal Skraup synthesis is claimed not to work very well with o-phenylenediamine, so arsenic acid is used instead of sulfuric acid. Could phosphoric
acid be substituted?
Amateur NMR spectroscopist
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