Amfetaminesynthese van P2NP via Al/Hg (video)

[Marvin "Popcorn" Sutton]

Mijn ervaring is dat aluminiumfolie de beste vorm van aluminium is voor amalgaam. De belangrijkste voorwaarde is dat het geen vreemde componenten bevat, alleen 99,9% Al. Poeder en korrels aluminium zijn ook geschikt, maar het wordt aanbevolen om ze in grotere hoeveelheden te gebruiken voor de reactie en de opbrengst zal niet zo goed zijn als bij het gebruik van folie.

 

[waltjr5858]

I'm not sure 99.9% foil exists. We'll it does and i believe it's labeled 4n and 5n aluminum. Which a roll of that stuff cost at least 2 to 3 hundred possibly more... anything on Amazon or ebay is going to be 98.5 at best like regular renyalds wrap

 

[nofuckups]

I had a failed first attempt and kinda fucked up big time by inhaling toxic fumes from the violent reaction.

As I poured the P2NP solution into the flask, the funnel on the flask couldn't hold itself and started bouncing (simply because of vapor pressure from the reaction). It happened so quickly that I couldn't find any time to process what's happening and to put a condenser. As a result, I inhaled some toxic fumes from the reaction and I'm not exactly sure how toxic they were but it smelled so bad. Some solution got spilled as a result and the reactants got evaporated in the early stage.

The yield from my 10g setup was like 300mg of white salt(turned out it was some basic byproduct or unreacted amphemine freebase). It tasted like a soap and had a burning sensation so I threw it away. 5-6% yield was a red sign anyway.

Some mistakes that I made that newbies can avoid:
1. Don't use a small funnel on flask: When pouring the P2NP solution in the amalgam, make sure your funnel's stem is big enough (especially w/ a >=10g setup). Smaller stem/funnel size in general can be a bottleneck and cause spillage or other adverse outcomes (you have to be very quick here to add a condenser and shake the flask).

2. Make sure you don't evaporate the solvents in the P2NP+IPA+GAA solution while heating it. Sometimes P2NP crystals may not dissolve so gentle heating may help(40-50'C) but if you heat it more then solvents like IPA would begin to evaporate and you'd lose solvents.

3. Ensure that your water is distilled and has close to zero TDS. I bought some "destilled water" bottles but they turned out to be just purified water with a 25-30 TDS. It's not a significant issue but contaminated water should be avoided in the amalgam phase to avoid unnecessary reactions with water impurities.

4. Properly acidify the amphetamine freebase before proceeding for drying. My pH papers were shit so I couldn't measure properly but you shouldn't stop before a pH of 6. Keep adding more acid solution until you reach it. Mistakes at this stage can result in a basic soapy product, not amphetamine sulfate.

5. Extract your amphetamine freebase with a non-polar solvent. The video doesn't include this part but it's an important step to not miss if you want a successful and pure yield. Something like Toluene could work. I haven't tried this it before but next time I'm going to do this.

6. If it's your first time, be very careful with the exothermic reaction when adding P2NP solution to the amalgam. In reality it can be far more violent than what's shown in the video so be prepared for that. Proper PPE and preparation can help like keeping cold water and condenser handy.

---

I have a few questions here for the experienced chemists:
1. How to deal with solvents volume loss? Even after a condenser and ice-baths, sometimes it can evaporate more. At what stage are we safe to add some IPA to the mixture? The video descriptions says you can add some IPA after the reaction is complete(to rinse the flask). Is that correct and if yes, how much are we talking at this scale? 15-20ml?

2. Can we add the P2NP solution slowly and in batches instead of at once? I can see this can result in more solvent evaporation but I really want to avoid overheating and violent reaction.

 

[waltjr5858]

I am having a problem getting the timing of the amalgam down to get to that very reactive state. It does react and the foil completely dissolves but I get ton of failures. The only ones that work are the ones that react violently right from the get go. Do you have any pics or anything of when to pull the trigger and the amalgam is ready. My aluminum starts to dissolve on the edges and the face of the aluminum doesn't look ready. I clean it throughly the aluminum and give it a quick run in 1% hydroxide to remove any oils. Or sometimes I don't... same result. I am using liquid mercury ii nitrate made from instructions on this site. I am going to try some more reactions with grains....

 

[nofuckups]

That's been my experience with two experiments so far. Either my amalgam isn't good enough or my p2np reduction is incomplete. The end result for me is always some byproduct or unreacted junk instead of amphetamine sulphate. It does look very white, fluffy and water soluable though. Heck, even pH is similar to amphetamine sulphate but when I run some tests like burning it with a lighter flame or dissolving it in a warm IPA solution, it stays solid and doesn't evaporate/dissolve. Also the taste is either mildly salty or soapy.

I'm gonna extract with Toluene next time.

 

[NieDoswiadczony]

and if I use 99% acetic acid and do not add water, will the reaction be bad?

 

[golab071]

The aluminum amalgam needs some water to function effectively because the reaction Al + H⁺ → H₂ proceeds faster in the presence of water.

In a completely anhydrous environment of IPA + 99% acetic acid, the reaction may slow down or not start at all.
Have you already tried carrying out the reaction? How’s it going?

 

[nofuckups]

how much water exactly? Isn't the leftover water on foil after rinsing sufficient? I use >99% GAA and IPA so I'm wondering if i should add some water to this solution. For a 10g scale, what quanity of water should be added if any? Do we actually need to add water if the foil is wet?

 

[waltjr5858]

Hydrogen actually is bad for the reaction. The reaction takes place on the aluminum surface with the mercury mediating the electron transfer. There's also something else happening to do with protons and a radical something but I forgot the rest. But... hydrogen is coming no matter what obviously.

 

[NieDoswiadczony]

after the reaction of Al with P2np I added NaOH and 2 layers separated but I did not reach pH 12, can I add NaOH solution again to reach pH 12?

 

[GhostChemist]

Yes, you can add an additional portion of NaOH

 

[Johnny Ringo]

Hey guys I want to do this synthesis on big scale in a barrel. In my theory I want to do the amalgam in a seperate bucket with aluminium sheets and then transfer it to the barrel and add the p2np so I can wash the mercury before I start the reaction.
Are there any complications I should look out for or overthink something?


I need at least 3liter oil per synthesis how much p2np would I need for that?

I have some experience with this synthesis and I know what to expect approximately but the result was every time a bit different in terms of yield. For example from 10g I got around 70ml but with pretty high ipa proportion. Then I went up to 25g and I'm pretty sure its because I cooked it with more heat and experimented a bit with the cooling it came out less than with 10g. My theory is its because the ipa evaporated more than usually.
Also I ask myself if its good or bad to dont cool that much like the quality from both runs was solid but when I didnt really cool it the temperature stayed longer stable what should be a good thing right?

Hope somebody here can enlighten me a bit.

 

[waltjr5858]

I would start very small first many times over... this reaction can be finicky and it is beyond easy to lose all precursor... that would suck. A lot of people have had all kinds of issues but once you get good at it I'm sure you could pull it off on a larger scale. Also the aluminum used is fairly important. Regular cheap aluminum foil will most likely result in a failure. Certain alloys are way better suited for this like 1050 or 1100 or if you really want pure stuff 4n or 5n but those are super expensive but very very pure aluminum. I know about the failures intimately and have had tons of them lol.

 

[waltjr5858]

I would start very small first many times over... this reaction can be finicky and it is beyond easy to lose all precursor... that would suck. A lot of people have had all kinds of issues but once you get good at it I'm sure you could pull it off on a larger scale. Also the aluminum used is fairly important. Regular cheap aluminum foil will most likely result in a failure. Certain alloys are way better suited for this like 1050 or 1100 or if you really want pure stuff 4n or 5n but those are super expensive but very very pure aluminum. I know about the failures intimately and have had tons of them lol.

 

[NieDoswiadczony]

hello I have a question about Al/Hg synthesis if when adding sulfuric acid flakes form does it mean everything went well? or if something was wrong in the synthesis will flakes also precipitate

 

[GhostChemist]

it is advisable to always check the product by tests
as for amp

 

[waltjr5858]

That means at least some form of your reaction is an amine so yes that's good but... that doesn't mean that the double bond was also reduced. The only way to verify if the double bond was reduced that is very simple that you can do at home is to react some of your product in its free base form so before you do the salt thing with sulfuric acid take your oil and put a small amount of that in a nonpolar and then add some bromine to a separate beaker containing the same nonpolar and start dripping some of your product in nonpolar into the bromine with nonpolar just small amounts maybe 10 mL of each total with the nonpolar and if the color of the bromine disappears the double bond did not break and you still have an alkene. There are other ways to verify but that one is ridiculously simple.

 

[NieDoswiadczony]

I have a problem with bromine, there is another way to do it at home

 

[NieDoswiadczony]

what is the way to check the free base of amphetamine oil -A whether it is good and whether the synthesis was successful