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Author: Subject: Alternative to toluene, inert with acetylacetone
Technetium99
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[*] posted on 11-1-2024 at 08:08
Alternative to toluene, inert with acetylacetone


Hello,

I need to synthesize lanthanide acetylacetonates but because I want high purity and no hydrated/solvated form I will follow the metal acetylacetone route, simply reacting powdered metal with liquid complexant in a solvent and here there is a problem: I know that toluene is inert enough but the boiling point is too high, it will be evaporated and 110C° is too much for the complex.

Common solvents like alcohols and ethers are unsuitable because they are lewis bases and adducts will form.

Which solvent would you use in this context? Are alkanes like hexane miscible with B diketones? BP best below 80C°
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RedDwarf
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[*] posted on 11-1-2024 at 13:15


Vacuum distillation?
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DraconicAcid
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[*] posted on 11-1-2024 at 13:19


Or just let it evaporate at 80 C. It won't boil, but will slowly dry up.



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clearly_not_atara
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[*] posted on 11-1-2024 at 16:18


Is acetonitrile applicable? It complexes but is easily displaced by other ligands.



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Technetium99
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[*] posted on 18-1-2024 at 08:30


Thank you all, at the end I did some more research, I found a paper where they synthesized ammonium compound by bubbling ammonia through a solution of acetylacetone in hexane, so this solvent is ok. Acetonitrile will be plan B.
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