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Author: Subject: Phthalic acid synthesis
teodor
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[*] posted on 2-12-2024 at 02:02


I remeber one more point why I don't like permanganate. When its reduction is started it doesn't depend on the rate of your organic product oxidation. It just don't stop untill all permanganate is reduced (not because of the organic oxidation). I believe with CrO3 you can see the actual rate of your compound oxidation (the change of the color).
You can easily get any (di) chromate from CrO3 in situ, but CrO3 is not always a substitution for dichromate for acetic acid solvent because it doesn't dissolve in AcOH as good as dichromate. So you have to mix NaOH with it in a small quantity of water before AcOH addition in this case.

[Edited on 2-12-2024 by teodor]
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Keras
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[*] posted on 2-12-2024 at 22:53


I have no personal grudge with permanganate. Is just that it is difficult to source because it’s listed as a drug precursor over here in the EU. So you have to make it yourself from manganese oxide by the fusion process, which takes time.



[Edited on 3-12-2024 by Keras]
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[*] posted on 2-12-2024 at 23:20


Quote: Originally posted by Keras  
I have no personal grudge with permanganate. Is just that it is difficult to source because it’s listed as a drug precursor over here in the EU. So you have to make it yourself from manganese oxide by the fusion process, which takes time.


In the UK it is sold on eBay, Amazon, APC Pure and several other sites.




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teodor
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[*] posted on 3-12-2024 at 00:51


Quote: Originally posted by Keras  
I have no personal grudge with permanganate. Is just that it is difficult to source because it’s listed as a drug precursor over here in the EU. So you have to make it yourself from manganese oxide by the fusion process, which takes time.
[Edited on 3-12-2024 by Keras]


But you need it in the form of solution. So, you can try to use manganese sulfate + ammonium persulfate (as you planned) + silver nitrate to generate it in situ during the synthesis.
Check this thread: https://www.sciencemadness.org/talk/viewthread.php?tid=15996...

Because the synthesis will consume the permanganate there is a chance it will go to completion.
Also the rate of permanganate generation can change the synthesis, but probably it would be interesting to try. As I said, the problem with permanganate is that it can be reduced faster than the organic compound to be oxidised.
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[*] posted on 3-12-2024 at 12:13


Lol, turns out I might’ve made manganese sulphate inadvertently. During my last experiment with naphthalene and potassium permanganate, I collected the cake obtained after reaction and filtration, which contains mainly manganese oxide, and added in it sodium hydrosulphite. It immediately cleared up and I’m now with a beaker full of a whitish powder in water. That might be it. I’ll filter it tomorrow and see.
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