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Author Topic: Requirement of glacial acetic acid and water in same step?  (Read 66 times)

Impossible

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Requirement of glacial acetic acid and water in same step?
« on: April 27, 2013, 04:38:23 AM »
I shall preface this by saying that I have extremely limited knowledge of chemistry, however I am learning quite well as I peruse old archives and patents.

Following diacetyl's(I've seen identical methods posted by others so I'm not sure if he is the original author) Al/Hg reduction of P2NP to amphetamine, I see that he calls for GAA to be mixed with water several times throughout.  This seems somewhat counterintuitive to me.  Is it feasable to simply use acetic acid to the conc. described without specifically using anhydrous?

i.e.
Quote
Mix 50ml of the GAA with 25ml of Distilled Water in flask
Instead, start with 66% acetic acid, using 75ml.



Glacial acetic acid is quite difficult to source where I am(as well as H2SO4, so sodium acetate + H2SO4 is not really an option either) so I am attempting to find some workarounds.

fishinabottle

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Re: Requirement of glacial acetic acid and water in same step?
« Reply #1 on: April 27, 2013, 10:51:24 AM »
70 to 80% acetic acid is the solvent in this reaction.

Those who use GAA and add water do so because they have it.

You MUST do an acid-base extraction or at least a steamdistillation at the end. Just using the alcohol-layer and make the salt from this WILL carry mercury salts into your product.

/ORG

Impossible

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Re: Requirement of glacial acetic acid and water in same step?
« Reply #2 on: April 27, 2013, 12:56:08 PM »
Yes... Luckily both an acid, and a base, is still within ones ability to procure in this country, otherwise it'd be a sad little state of affairs. H3PO4 will likely be the substitute for H2SO4 when converting freebase. 

Thank you for your help.  I'll be posting a feasable method to mass produce ephedrine as a more worthwhile 'thankyou' when I wake up :).
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