dermolotov
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Synthesis of Aluminium Phenoxide
I can't find any current methods of this synthesis at the moment. The only one came from an old manual that I've now lost that called for 0.001 mol%
Mercuric Chloride, 1 mol of Al, and 3 mol of phenol in a nitrogen atmosphere.
My guess nitrogen is just a regular procaution and it need not be completely dry or devoid of oxygen? Should it be easy as adding Al powder to phenol
and refluxing for 5 hours?
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dermolotov
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Addendum: I should mention that gritted aluminium is one of the biggest wastes of money if I can just use Al(OH)3 instead.
Would that be easier or harder to react with phenol?
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gdflp
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This link makes no mention of the nitrogen atmosphere so it may be unnecessary. The mercuric chloride is present to remove the oxide layer from
the aluminum and increase reactivity by forming the Al/Hg amalgam. Refluxing aluminum powder and phenol may work, but the yield may be significantly
reduced by excluding the mercury catalyst.
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dermolotov
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Ah! Brilliant. This was the exact pdf that I found a few days ago. For some reason, I couldn't find it today.
It does mention the Nitrogen atmosphere, though. But it isn't mentioned anywhere besides experimental. Plus, I don't think oxygen or water would
interfere [much].
For those keeping track at home, here's the procedure from the journal:
| Quote: | | Al (1 mole) was added to excess phenol (4.3 mole), in 2 L dried THF (solvent) and (0.001 mole) HgCl2 in a flask [9]. The mixture was refluxed for 24
h under a N2 atmosphere with stirring. Solvent and alcohol were removed by vacuum distillation. Aluminum phenoxide was not extracted by further
vacuum distillation since it decomposes on heating and was collected from the flask |
Quote: Originally posted by gdflp  | | The mercuric chloride is present to remove the oxide layer from the aluminum and increase reactivity by forming the Al/Hg amalgam. Refluxing aluminum
powder and phenol may work, but the yield may be significantly reduced by excluding the mercury catalyst. |
This is a shame. But I would much rather lose yield than add mercury to my compound. Just not worth it for me...
Last mentions:
1. Would Gallium create the necessary amalgam? Would it theoretically work as a catalyst as well considering reflux temperature?
2. Will try using toluene as the solvent. I expect no possible loses on that front.
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gdflp
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I can't answer definitively, but this thread may be of some use http://www.sciencemadness.org/talk/viewthread.php?tid=31127
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dermolotov
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Will skim it and prepare a method. Report back soon with results.
Cheers GodFlip 
Won't think many people will make use of this reaction/product. But then again, who the hell is making use of my thesis? 
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CuReUS
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| Quote: | | Would Gallium create the necessary amalgam? |
Al-Ga amalgam is so powerful that it can liberate H2 from plain water,so I think it should work,although Gallium is expensive so it is not
as common as Hg
https://www.youtube.com/watch?v=JasZ8V6LpbQ
https://www.youtube.com/watch?v=PqDU6DsYr98
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CuReUS
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I was wondering,what would happen if AlI3 is reacted with sodium phenoxide,will it form aluminum phenoxide ?
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