Is there a reason Sulphate salts are preferred for amphetamines

[Mo0odi]

I mixed acetone with sulfuric acid
There are no impurities in it, it is a great product

 

[BrownRiceSyrup]

no hes right, its this white kind of stringy shit. doesnt seem to dissolve in water. If you leave sulfuric in acetone long enough in high concentrations it also turns red.... least it did with me...

 

[diogenes]

I had a long period of trying to get Acetone-Sulphuric acid mixture for salting, and the only way to prevent the formation of mesilates (red colour and awful smell) was to use freezer cold acetone and acid, but even with the utmost care it would turn red after a while (couple of hours). My experience confirms what w2x3f5 says that sulphuric acid-IPA mixture is much better for salting.

 

[OrgUnikum]

Amphetamine mono-Phosphate must be prepared by titration in water, the ph you want is 5 to 6. Monophospate cannot be prepared in alcohol as when one adds the phosphoric acid 75 or 85% doesn't matter, as is or in alcohol to the base in alcohol there comes the point when the all the Amph turns all of a sudden into bubblegum and it does not take on any acid anymore. So you have a mixture of polyphosphates . It is no problem to dry this bubblegum mass and it gets dry without problems and it can be consumed and its not bad but not the mono-phosphate.
The monophosphate which can be made by adding water and then diluted phosphoric acid to the base in a non-polar solvent and then mix the holy shit shit out of both, has the advantage that it is much more water-soluble then the polyphosphate and also more then the sulfate. This higher solubility means a better bio-availability and it has a slightly faster onset then the other salts. Only the carbonate salt is said to beat it, but I never tried to make it.

Now when you make the monophosphate in water something happens what will disturb you first: When adding the phosphoric acid you will first see salt falling out of the solution and this will make you happy. When adding more acid all of a sudden all the salt will -puff! - disappear again! In difference to sulfuric acid where this is bad, it is exactly what you want with phosphoric acid salts as you want the one with the best water solubility. Which you get at ph 5 to 6 and after separating and evaporating the water.

Red discoloration which appears when adding too much acid is not caused by acid or amphetamine but by impurities, mainly P2P and mildly basic impurities which came through the process. P2P goes nicely through steam-distillations and A/B procedures as it is amphoteric in the presence of bases and acids, in special with bases, say it becomes suddenly water soluble to a far wider extent.
Really clean Amphetamine base does not change color no matter how much acid you add. None of the post-reaction protocols I have seen here produces really clean Amphetamine base and so the reading about the discoloration (from pink to red) problem is no surprise at all.

 

[41Dxflatline]

This is at odds with the procedure listed in Pharmaceutical Manufacturing Encyclopedia which uses alcohol but it absolutely fits with all of my practical observations. The salt also does a disappearing act in IPA too from the water in the H3PO3 which is when I stop adding acid. Also, good to see you still posting after all these...decades.

 

[w2x3f5]

H3PO4 bro )

 

[w2x3f5]

acetone works much better, it turns out a good solid salt, without snot. I personally checked back in 2005)))

 

[w2x3f5]

Regarding p2p and coloring, I will support. this is true. Impurities of p2p and its derivatives give color due to by-products, this is also the case for p2np and p2p syntheses, the amine after fractional distillation in high vacuum does not color when using an excess of acid, the pure base of the amine is completely colorless and transparent.

 

[OrgUnikum]

Well possible that you can make the mono-phosphate in Acetone, I never said the method I described is the only one.
But for curiosity, why "much better"? In my eyes its at most a question of personal taste what method one prefers.

 

[w2x3f5]

ease of preparation and isolation, amine phosphates are very poorly soluble in acetone, easy dry.

 

[OrgUnikum]

You are nicely explaining why adding H2PO4 to amine base in acetone will NOT give the monophosphate salt. As theamine will drop out as the more insoluble salt consisting of phospahes comprised of one ohosphoric acid molecule and several amine molecules, this salt will not react further no matter how much more H3PO4 you add.
Monophosphate means exactly one molecule of amphetamine to one molecule of phosphoric acid and thats not to achieve by the by you described method.

I will not stress this further, thats my final comment on the matter, do not have nerves nor time for this, sorry.

all the best, good luck and happy cooking!

 

[w2x3f5]

I used this method in 2005 and it proved to be excellent. it is your own business to happen or not. This is my practice and several laboratories. Good luck on your difficult journey. Monophosphates, unlike other phosphoric and amphetamine salts, are very poorly soluble in acetone.

 

[Pervitin]

I read the thread and to revenue what you said in simple steps,
If I had pure steam distilled Amphetamine base, like 100ml. How much solvent do I need and witch kind of?
Acetone would not work when I use H3PO4 and how much Phosphate acid I have to drop into?

i don't want someone to do the dirty laundry, but it would help me to understand the process, with a specific example, thanks.

 

[Gordon Ramsay]

If your goal is to crystalize it you can go and mix it with acetone or methanole where I would recommend Acetone to then drip it down to salt with sulphuric acid

 

[Pervitin]

Thanks, so I have to mix the pure base with like 1:1 dry acetone and then drip my 85% H3PO4 in it until it reaches PH 5-6? I doesn't understands @OrgUnikum post "The monophosphate which can be made by adding water and then diluted phosphoric acid to the base in a non-polar solvent and then mix the holy shit shit out of both, has the advantage that it is much more water-soluble then the polyphosphate and also more then the sulfate." When I have to add water. I thought water and A-Oil effect the yield? And how much water?

 

[Gordon Ramsay]

You can follow the last steps here

One-pot amphetamine synthesis from P2NP with NaBH4/CuCl2 (1kg scale )

There are many different options to produce the amphetamine salts but you can simply follow this guide

 

[Mohammed_Lee]

Hello and first of all a big thank you for the active members of this forum. I would't have gotten to the point I am without you!
My problem: I got enough (old) sulfuric acid for exacately one batch. The problem is that during time it got a yellow colour. Can I use this? (I I cant get my hands on new one atm)
But I got enough phosphoric acid @orgUnicum:

"The monophosphate which can be made by adding water and then diluted phosphoric acid to the base in a non-polar solvent and then mix the holy shit shit out of both, has the advantage that it is much more water-soluble then the polyphosphate and also more then the sulfate."

Can you tell me the the mix ratio Water:Base and Waterhosphoric acid? Also I got n Hexan is it suitable as a non polar solvent?

best regards

 

[Mohammed_Lee]

I have another question concerning my first self made batch (propably not) amphetamin phosphate and decided to post it her instead of opening a new thread. I made it via P2NP HgCl Method and everything was looking good. The Amalgam; the reaction after adding the RM. The only thing I did wrong was the temperature controll during the reduction (I think I let it get to hot sometimes. But after 24h I got 2 nhice layers decanted the upper one and seperated the last bit wit a separatory funnel.
Long story short I enden up with 85 g of whatever (from 10 g P2NP). If anyone has any Ideas what went wrong and how I can avoid this I'd be verry glad for an answer. right now I'm making my second Batch where the amalgam part didn't work out that well (first time with cofffegrinder wich broke during the process.
Also If anyone has an Idea about the questions in my last post: please let me know.. I have to finish a third Batch until Monday Morning because I registered it for analysis and want at least one sucessfull batch.

thx in advance,
lee

 

[w2x3f5]

You got a mixture of inorganic salts, so I don't see any mention that you used alkali to get the amine free base. You don't know what you're doing, it's dangerous.

 

[Mohammed_Lee]

No, this should only be a short summery since I had a bit of stress. I followed the viedeoguide and spent hours in this forum reading post about this synthesis. to be accured: I of course but the mixture in a beaker, waited ~20 and then added a NaOH sollution until I reached ph 11 (would I get 2 layers without the alkanisartion?)
Any Ideas what went wrong?

 

[Mohammed_Lee]

Does anyone have an idea wich mistake could have caused this? in whitch step of the synthesis did I make a mistake?

 

[w2x3f5]

Write in detail what you did, what reagents you used, what you observed. how can we understand you if you give small pieces of information.