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Author: Subject: Anhydrous aluminium Chloride and more!
XeonTheMGPony
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[*] posted on 10-6-2021 at 15:25
Anhydrous aluminium Chloride and more!


Well My anhydrous aluminium Chloride finally arrived, paper disintegrated on packaging and stickers discoloured, oh boy not good signs!

So on comes the dehumidifier and let that run for an hour to dry the lab out, I sieve it, I recover 3 portions.

Portion 1, Anhydrous and good appearing quality, not much but enough.

Second portion is discoloured yellow, obviously damp with some fuming of HCl that is int he brown bottle

Third portion dam right damp and clomped it is int he 2 smaller bottles.

Now my next question is I need to make ChloroBenzene for my DDT Synth, How sensitive is this to moisture? As if possible would like to be able to put the slight damp stuff to work so it isn't total loss!

IMG_20210610_171041.jpg - 1.3MB
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paulll
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[*] posted on 10-6-2021 at 18:21


Is there an advantage to using Aluminium chloride in this synth? I'm looking at it myself in the very near future, but with ferric chloride.
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[*] posted on 10-6-2021 at 19:19


Ferric chloride is a milder catalyst, but one would think that chlorine is reactive enough that it wouldn't matter.



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[*] posted on 10-6-2021 at 23:07


The affected anhydrous AlCl3 is not really damp. Water and anhydrous AlCl3 cannot coexist, they react violently, producing Al(OH)3 (or some basic stuff like Al(OH)2Cl or Al(OH)Cl2) and HCl. I can imagine that any basic material in your AlCl3 does no real harm in your reaction. Only thing is that it adds extra crap to be separated from your final product. Good thing is that this crap will be insoluble solid stuff, which easily can be separated.



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unionised
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[*] posted on 10-6-2021 at 23:45


I seem to recall that AlCl3 is one of the chemicals you can purify by sublimation.
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paulll
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[*] posted on 11-6-2021 at 01:55


And then I saw ...
https://www.youtube.com/watch?v=G_4kfY0dR2A
(From toluene + TCCA)
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XeonTheMGPony
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[*] posted on 11-6-2021 at 03:42


So the clumpy stuff should still be useful in the ChloroBenzene synth? what would be the wet behaving like material then? As when I ground it it behaved like most slight damp powders do by sticking to its self and .

The person who shipped it tried to seal it good by using hot glue, I have experience with that side of things and hot glue is deceptive, when first done it appears to be good seal then when you tune your back it separates from the glass surface!

So by the time it arrived (All most 2 months) enough had reacted to destroy the shipping paper and label totally destroyed
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[*] posted on 11-6-2021 at 11:45


The chlorobenzene does not need AlCl3. The ferric chloride catalyst can be generated in situ, a piece of steel wool is good enough.
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[*] posted on 12-6-2021 at 03:38


Generally when making bromobenzene a few grams of aluminium or iron powder is all it takes: https://m.youtube.com/watch?v=H2WV52P3eus
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[*] posted on 12-6-2021 at 05:36


Putting aside the issue of whether you need aluminum chloride to make chlorobenzene (you don’t) my gut feeling is that the slightly damp but still powdery stuff in the brown jar is probably good enough to use, but I wouldn’t trust the really wet and clumpy stuff. Use the best stuff when you need to be certain it will work, like when you have very limited quantities to work with, or valuable reactants.



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clearly_not_atara
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[*] posted on 12-6-2021 at 07:09


You can monochlorinate benzoic acid in alkaline aqueous solution with hypochlorite. Since you're likely dry distilling to make benzene anyway, this sounds a lot easier than acid-catalyzed chlorination with chlorine!

https://www.nature.com/articles/131028d0




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 12-6-2021 at 07:40


Anyone have any idea how to get a fair amount of 1,2 di halogen product rather than 1,4dihalo compound?
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[*] posted on 12-6-2021 at 07:45


Quote: Originally posted by clearly_not_atara  
You can monochlorinate benzoic acid in alkaline aqueous solution with hypochlorite. Since you're likely dry distilling to make benzene anyway, this sounds a lot easier than acid-catalyzed chlorination with chlorine!

https://www.nature.com/articles/131028d0


If U chlorinated benzoic acid first then dry distilled with naoh to get the benzene
U would form a phenol by the action of hydroxide exchange with the chlorine forming salt as a byproduct.
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[*] posted on 12-6-2021 at 08:18


Quote: Originally posted by draculic acid69  
Generally when making bromobenzene a few grams of aluminium or iron powder is all it takes: https://m.youtube.com/watch?v=H2WV52P3eus


Thanks, I do have steel wool I will use for the Bromination.

I plan to buy some ground aluminium, Iron, Zinc, Tin.
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XeonTheMGPony
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[*] posted on 12-6-2021 at 08:21


Quote: Originally posted by clearly_not_atara  
You can monochlorinate benzoic acid in alkaline aqueous solution with hypochlorite. Since you're likely dry distilling to make benzene anyway, this sounds a lot easier than acid-catalyzed chlorination with chlorine!

https://www.nature.com/articles/131028d0


I have a Bottle of clean dry distilled benzene on my shelf lol, I am making ChloroBenzene to make DDT

The Chloral hydrate synth is done, and all wastes processed and disposed of, So now time to learn as much as I can about the next process ie Chlorination and Bromination of Benzene.

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