Microwave rocks, Dude 😎

[Jesse_Pinkman_]

I visited a friend today, let us call him SWIM
He tried an alternative way for p2np, by Microwave, on basis of instruction of William Dumpler.
Microwave variant:
1. 100 ml benzaldehyde, 100 ml nitroethane, 25 ml glacial acetic acid and 20 ml n-butylamine was added in 500 ml glass.
2. Put a rubber glove on a glass.
3. The glass was put in the microwave.
4. Turn on the power of 750 W and warm so much time so that the mixture does not boil.
5. We repeat the step 4 several times, let me cool the mixture. Minimum 6 irradiations.
6. After that, add 100 ml IPA, stirred and put in the freezer for 12 hours.
7. After that time, P2NP was crystallized.
8. Filtered and dried.

But the crystals were formed immediately after putting the 2 solutions together. SWIM used 2 beaker parallel, after every irradiation (6 times), he put the beaker into cold water for some time, 1-2 minutes, before next irradiation. At the end, he was able to turn the box upside down without any moving of the substance, still before putting it into the freezer...it was amazing and now he will wait till next day for filtering and drying.
What do you think?! Looks good?
I am not experienced but think it worked well, even if the solution boiled while first irradiation (730W, after aprox 1 min), so you have to watch the glove all the time.
If it blows up, switch the microwave off and cool the beaker.
That was his first time ever he did something like this, but it was a nice to see... tomorrow he will try to produce aluminium amalgame by using gallium and if it reacts with the p2np. Its just a tryout, because there are less experiences out there so far. If it works, it would be an awesome alternative to Al/HgCl2.
I will keep reporting about it, if it works.

 

[Jesse_Pinkman_]

This is, what i found for Al/Ga reductive amination of ketone via Gallium/Al + amine:
To the aluminum amalgam there was added 295g methylamine hydrochloride dissolved in 300ml hot water, 750 ml isopropanol
700ml 25% aqueous NaOH,197.5g ketone and finally 1750ml isopropanol. Hydrogen was vigorously evolved from th
aluminum amalgam, and the temperature of the solution rose quickly. The reaction rate was controlled by immersing the reaction flask in cold water during 2h, whereafter it was allowed to stand at room temperature with magnetic stirrin
overnight, with attention being given to the reaction mixture during the first hour so that the temperature did not ris
over 50°C

Aluminum gallium amalgam pre
The gallium amalgam is an excellent substitute in an al/hg reductive amination procedure. it's non-toxic, and stronger
A search of the internet will reveal, a patent where it has been used already to reduce NO2 and NH2. gallium is also
easily sourced. If you wanted to make a Ga-Al alloy, simply gently heat the Ga (m. pt. 29.7646ºC) until it is liquid, an
it will start to readily form an alloy by dissolving the Al. However, the resulting amalgam will have a higher meltin
point than the liquid Ga, so you would have to keep heating the mixture until all the Al is dissolved. In a 10,000ml
wide-mouthed flask, 190 grams of aluminum foil cut to 3x3cm pieces was amalgamated with 5grams gallium in 7000ml
warm water until the solution became greyish, and hydrogen bubbles was evolved in a steady rate from the aluminum surface. The water was decanted off, and the aluminum amalgam was washed with 2x5000ml cold water.

I think it could also be used for reductive amination of p2np.
What do you think?
Ga can be re-used and its very cheap.
50g about 40€.

 

[KokosDreams]

Nice dude!

 

[MadHatter]

The gallium idea has been tossed back an forth for some time. It's worth trying. But I wonder how you're going to get the gallium to interact with all the aluminum without turning it into a salt first and dissolve it in water? Gallium forms blobs when melted much like mercury, and if you pour it in a beaker with a lot of aluminum strips the blob will just touch and interact with a portion of them.
If one instead dissolve the Ga in HNO3, forming Gallium Nitrate, one could dissolve that in water like the mercury nitrate, and then add that solution to the aluminum strips. Savvy?

 

[Jesse_Pinkman_]

That Video shows how to do it...
But if it doesnt work so well, SWIM has some HNO3 in his chamber.

 

[MadHatter]

Yeah, the gallium discussion is not isolated to this forum, naturally. It seems it produces inferior yields, at least that's what users report. Something with the electron donation capacity of mercury vs gallium. But still, more experimentals must be made, so go ahead!

Login

Login

www.thevespiary.org

Right now I have no P2NP at hand, or I would try it myself.

 

[Jesse_Pinkman_]

So, SWIM really had some issues with the Gallium, but finally it worked somehow. It was his first attempt ever in doing this kind of work, and became a little confused at the end with the seperate layers(DCM) and one time, instead of DCM, he grapped the sulforic acid and put it inside a beaker. It was a real mess, the solution did a jump and everything around 40cm was covered in shit
A separatory funnel just broke into 2 pieces.
But, after all, 50g p2np created 35g amphetamine hcl (his opinion), after washing and vacuumed with acetone. But even after hours, the smell of acetone did not disapper, so he decided to wash and dry with ethanol, and he is sure, that was not the best thing, because after that, there were no crystals anymore. Just a paste which dried very heavy after +6 hours. There were 25g left of a white, light greyish powder.

 

[Jesse_Pinkman_]

SWIM had a ph gauge but it did not work anymore...so everything was like, OK just try and hope for the best...He asked himself, why the solution became so darkred?
Does anybody know?

 

[MadHatter]

Great job! But ...

Amph HCL? Surely if you used sulphuric acid you'd have gotten amphetamine SULPHATE, no? If you had the hydrochloric salt it'd all be a gooey slurry mess. Red colour is often a sign of over-acidification.

And why did you use DCM, and in what stage? Try doing your write-up more systematical so it's easier to follow.
Like so: "1. 50 g of a P2NP was dissolved in 100 ml of IPA and then added to gallium amalgam. Upon addition, heat was evolved with a peak temperature of 80 C ... ". This is how you describe lab work, and it's done this way for a reason. Right now it's very difficult to understand what you did and when.

And how did you produce your amalgam in the end? I'd love to see a proper write-up of that too.

Did you try the end product? Is it working?

This is a very interesting take on the procedure and I for one would really like to see it properly described! It would be very valuable.

 

[Jesse_Pinkman_]

Yes, you're right...
At the beginning of all, there was the microwave procedure to create p2np, but yield was not so big as expected, washed with Xylol several times, first run 116g, the rest solution created new crystals over night in the freezer, +40g. SWIM expected over 300, what He had read in other recipes.

But ok, first time...no need to cry.

Preparation:
•50g p2np in 200ml warm ipa in beaker
•20g NaOH in 250ml distilled water in beaker (refrigerator after 10min)

•400ml glacial acid (100%) + 100ml distilled water in 2000ml flask
•75g Alu cut into squares about 1x1cm, but my opinion, better smaller If you use Gallium.(0,4mm thick, scratched surface from both sides with a screedriver)
•50g gallium (better use GALINSTAN!)
SWIM tried with 5g first, but reaction did not want to start properly, Alu was not small enough, GA did not had enough contact)
SWIM Mixed rest of GA with distilled and nitric acid, only had 38%.
GA and Alu we're in a 1000ml flask with heating mantle. Heat is absolutely needed if work with GA.
No heat, no fast reaction.
He needed some patience and a lot of shaking, shaking, heating, but then it began to dissolve, became grey and exotherm, about 70-80 degrees.
SWIM had some Alu left and threw small(small pieces) amounts into the flask, to let it run.
After 40 minutes he puts the water out of the flask and fills the solution of the 2 beaker (p2np+glacial acid) onto the Aluminium amalgame. But no heavy reaction, it was not so easy to keep the reaction ongoing, so some more alu pieces and some ethanol (50-100 ml several times). It helped to keep the reaction alive but not compareable to HgCl2.
The Alu was too big and maybe to thick for fast reaction.
But okay, the solution became dark, green and the alu dissolved more and more.
After aprox 40 minutes, he cooled the flask down in ice water and after that he putted the solution in a big beaker. The NaOH comes also in little steps, stirring after every time.
The recipe which SWIM had, included the usw of DCM to separate the solutions. But there was the time, when that mistake happened, when sulforic acid(98%) instead of DCM was used. After that, everything was strange and SWIM had 3 beaker, 1 with red, 1with orange, 1 with clear solution.
He sepatated them with a funnel. because of the accident with sulforic acid, some crystals showed up in the red solution, but normaly this was not the time either it was planned to do that. SWIM wanted to obtain the oil, the freebase completely.
SWIM worked from 15:30-04:00 o clock.
He was tired and only took the crystals, washed with acetone 3 times and some hours later with ethanol.
And normaly you get amp sulfate when using sulforic acid, thats right, but it looked so different, compareable to that, what comes to my mind, when i think on a.sul.
You see it on last pic
By the way: GA is non toxic so no need to wash the alu oder distill something

 

[Jesse_Pinkman_]

And yes, it works very good, but it has absolutely no smell, just taste is bitter but not bad...i think most consumers dont even know, that pure amphetamine has no real smell.

 

[MadHatter]

Thank you! So if I understand you correctly you converted the gallium to gallium nitrate before reacting it with the aluminum? By dissolving it in HNO3?
That's what I would do too. Keep in mind though that while not exactly toxic, gallium nitrate is bioactive (a medicine) and can lower your blood calcium levels. Not dangerously at low doses, but it should be treated with respect and properly cleaned out of the final product. Fully water soluble though, so an easy cleanup.

And you didn't make it easy for yourself by using these thick chunks of aluminum instead of foil. Why not just use ordinary aluminum foil? These thick plates will, as you say, slow down your reaction.

And DCM is a polar solvent, I'm not sure it will mix all that well with the amphetamine freebase oil? It tends to create a third layer. I'd rather use a non-polar solvent like petroleum ether or toluene.

 

[MadHatter]

Also, man, you use a lot of GAA! That's what makes your reaction mass over-acidify and turn red, I think. Also you'll end up with acetylated impurities that can make your salt all weird in texture, smell and taste. Ease up on the glacial. Also, if you only used sulphuric acid in the reaction you'll only get sulphate salt. I don't see any HCl mentioned in your text, so what would form a hydrochloride salt? I rather think it's that acetic acid that makes your salt strange.

 

[Jesse_Pinkman_]

Yes, absolutely...these chunks fucked up everything, but the roll of alu was 5m long and SWIM cutted it with a tong by hand...next time he will use alu grit instead this shit, but He thought, 0,4mm is better than foil.
It is possible to make Aluminium amalgame without solving in acid but it takes more time and better you keep the alu in touch with the GA, before put it into the flask or beaker. However, Galinstan should be perfect, i is composed of gallium, indium, and tin.
He will try it next time, just to proof the theory. But, we saw now, it IS defintely possible to use Gallium instead of these mercury shit, which is so problematic to dispose.
And yes, the product has been cleaned as good as is could, to get the best available quality. No smell, No burning nose, absolutely smooth and kicks ass

 

[Jesse_Pinkman_]

The solution with ga, water and nitric acid was removed and only the alu was put into the other solution...i dont think this was a factor. But next time things will be done better, it was the very first attempt, so from mistakes people learn.
And normaly 5g Ga is enough i think, but there were no written experiences with this kind of reaction with this ingredients. It was a mix of different recipes.

 

[MadHatter]

Ok, there seem to be a confusion of names here. Gallium metal is named "Ga" in abrevation (not "GA"), like in the periodic system. GAA = Glacial Acetic Acid. You use a lot of it. Ease up on the glacial acetic acid.

 

[Saul]

he had to take methanol than he had that fresh smell ;-)