One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[MadHatter]

Yes, I couldn't see why not either, so I tried. It seemed to work like a charm.
I can't testify to yield yet, but I do have a bottle of formylamphetmaine over acetone and MgSO4 standing in the fridge, waiting to be salted out. I need to concentrate and clean some sulphuric acid first though, I have no concentrated stuff lying around right now. Our work is never done ...

 

[MadHatter]

So I tried salting out a small amount with some sulphuric acid in acetone, and when the solution went neutral it also turned quite brightly green. There's a small layer of salt at the bottom, but it's not very much. Hmmm... I guess the green colour is from copper sulphate that's still in solution and that precipitates again when adding H2SO4? Or is there another explanation? pH is a perfect 6.

 

[WinterDust]

Hi Madhatter,

This happened to me once aswell, and it was because of faulty pH sticks.

So I over acidified the amphetamineoil.

Try new pH sticks, dip 2-3 sticks into the amphetamineoil, don't shake them when you take them out, put them on the table and let them rest for 30 seconds and check your pH value.

Best regards

 

[MadHatter]

Yeah? Well, the salt produced doesn't seem quite right either. It's too ... fluffy. More like needle crystals than amphetamine salt. Also, I did a small bioassay and it doesnt really seem to have any effect.

 

[WinterDust]

Needle crystals you say.

Did you have your amphetamine oil in the freezer or fridge over night?

Have you vacuumdistilled you amphetamine oil?

Best

 

[MadHatter]

Yes, it's been kept in the freezer diluted with anhydrous acetone, over MgSO4. It's clear but pale yellow. No, I didn't vacuum distill it.
But this was just a small portion of it I did as a test run, since the sulphuric acid I used was questionably dirty. I'm waiting for clean reagents though, I will probably use 85% phosphoric acid since that's accessible.

 

[WinterDust]

So,

The "needle chrystals" actually occur from the freezing of amphetamine oil without vacuum distilling.

If you go back in the thread you can see that I have posted about this problem but in the form of a jelly.

That jelly releases these chrystal needles but I dont know why they occur.

 

[MadHatter]

Sorry, I was uncorrect. It wasnt kept in the freezer, it was kept in the fridge, well below freezing temperature. And the final salt was vacuum filtered, so any freezing would have melted.

 

[MadHatter]

Sorry, I was uncorrect. It wasnt kept in the freezer, it was kept in the fridge, well below freezing temperature. And the final salt was vacuum filtered, so any freezing would have melted.

 

[MadHatter]

Also, something strange:
I saved the black slurry part of the reaction mixture, and combined it with the aqueous layer from the freebase separation. Poured in a bunch of acetone and left it standing overnight in a temperature just above freezing.
When I came to fetch it this morning there was the expected clear layer on top, but the bottom layer was SOLIDIFIED with clear, rock hard crystals. So hard the have to be chiseled loose. I tried solving some of them in tolune, acetone and water, but they're insoluble. The crystals themselves are clear as ice, but they.ve formed around the black nanoslurry of the CuSO4.
See attached picture taken into the beaker.
What on earth could this be?

 

[MadHatter]

After giving it some thought and a bit of experimentation, I'm pretty sure these are borate crystals. They dissolve just fine in warm acidified water.

 

[WinterDust]

@MadHatter, jesus christ this has annoyed me for a long time, but I can finally put it into rest.

You are correct, the "sludge" is borate crystals from the NaoH, I just did another reaction and the outcome was exactly the same.

Best regards

 

[WinterDust]

Hi,

So I made a smaller batch yesterday of 150g P2nP and extracted the amphetamine oil.

I put 0,5L oil in one pyrex beaker with plasticfoil on top with rubberband over it and 0,5L in a closed plastic bottle. Both were stored in the refridgerator over night.

The results were, the amphetamineoil in the pyrex beaker was still liquid and the amphetamineoil in the plastic bottle had crystallized.

Best Regards

 

[MadHatter]

Nah. I don't think the amphetamine oil crystallizes. I think it's borate crystals from the NaBH4.

 

[MadHatter]

So this was a total failure. I think it failed in one of the reductions. The first reduction is happening when P2NP is added, it breaks the double bond in the P2NP molecule. The second reaction takes place when the amine is formed, and is catalyzed by nanoparticles of copper from the CuCl2 solution.

In the write-ups I found on other fora it is recommended to add all of the copper solution at once, not dropwise. Also, I think it would be a good idea to add more NaBH4 before the addition of copper solution to aid in the second reduction, in case all from the first addition have been consumed by the first reduction and through reaction with water.

Thirdly, when the rm is brought to 80 C I think it's best to reflux the volatized IPA back to the flask, since it can bring with it any a-oil formed if the solution is basic.
I would then acidify the solution. When I did this reaction, the clear part of the rm was already in two layers, due to it being alkaline. You wouldn't want that just yet, so the addition of HCl until acidic will give one clear layer above the copper oxide layer.

I would then distill off the IPA completely, having the product locked into the water layer.

THEN I would add NaOH solution to the rm, creating an oil layer of product. This I would steam distill directly from the reaction flask into another flask, treat the water/oil in that flask with brine and then separate in a sep funnel. Finally, naturally, dry over MgSO4.
And then salt it out. And I'll be DAMNED if that doesn't work.

If needed, I'll add more copper solution and NaBH4, even heat the solution in the second reduction to get it going. Amination will happen.

 

[Hank Schrader]

Previously, when there were tons of nitroethane in the CIS countries, everyone produced huge amounts of nitropropene.
My colleagues at negative temperatures have learned how to obtain nitropropane with almost 93% yield.
Many experiments were done, and from 1kg (~6.13mol) of unsubstituted nitropropene, 941g (~5.7mol) of nitropropane were obtained.
As I said earlier, the stage at which propane is obtained is of great importance.
The more correctly it is done, the greater the yield of the final amine after reduction will be.
Propane itself can be reduced by any means, be it amalgam, zinc, electrolysis, Raney nickel at low temperatures, or palladium on coal.
The advantage of restoring nitropropane on amalgam is the scaling in many ways compared to nitropropene.
Today I will show you a method reduction of nitropropane with a yield of 60-65%

As we can see, propane. Propane is loaded into a solvent flask and a catalyst is added. Flask of three throats. The flask is equipped with a thermocouple, a reflux condenser and an auxiliary hydrogen supply.
Hydrogen is generated in the neighboring flask, which is supplied in small portions. (You can use a hydrogen tank.)
Every hour we take tests and see how the reaction proceeds.
When the analysis shows that the source material is consumed, the reaction is stopped and decanted from the catalyst.
Amphetamine is isolated without further purification.

The method can be improved and the amine yield can be much higher.
It is enough to make more excess pressure of 2-3 bar.
In general, the method can give 90% yield.

 

[MadHatter]

So in the spirit of a new year i wish to update my previous sad and tediious negativity,

I found some heavily diluted but clean sulphuric acid in the garage, and since I thought my reaction had gone to complete shit I figured "Let's mix this shit up, see what happens". You know, the fundamental theory behind all sound science.
So to that very suspicious 500 ml bottle of possibly amphetamine oil (or somethin) I've had standing in the fridge for a week was added ... well, enough weak-ass, water-polluted sulphuric acid to make it neutral. Slight clouding visible, but seemed to dissapear. Well, it's not like I had any hopes, said Ior The Old Grey Donkey.
In the fridge for an hour. When taken out, a transparent jello seemed to have formed in the bottle. Well figures, Ior thought again, all just shit. If Ior used the word "fuck" he'd be thinking "fucking polymerized piece of shit".
But I vacuum filtered anyway just to have a closer look at this gel. Could it be the cure for cancer?

But lo and behold!
Left in the Buchner funnel after sucking it off there was a solid thick layer of white, pasty precipitate. I scraped it into a crystallizing dish and let it dry för a little while. When I came back and stuck my nosy nose into the dish NOSTALGIA hit me like a KLF tune: it absolutely REEKED of that exact sickly flowery smell some really strong speeed used to have on the market in Europe. It got different names in different countries, but usually they all meant "Flower" anyway.

So now I actually got a bit interested and scientificcy. Had I made the contaminant that causes that disgusting flowery smell, or had I made flowery speed? (yes, I know thats speed WITH the contaminant in it. Plesae go away)

Relly, I didn't have any real drug reaction tests at home. Neither did I wish to wait any longer now for this goddamn son-of-a-bitch asshole pain-in-the ass batch. It was MIller Time.

"Well, cool cats die of curiosity, not old age" I thought and shoved half a smsll teaspoon into my mouth.
HORRIBLE, horrible horrible floral aroma and the usual bitterness of many chemicsls. Scientific note 1: I didn't die during the first minutes of ingesitng it. No organ seemed to critically fail.

So bioassay:

1. 8:22 PM. Half a teaspoon of disgustingly floral-smelling unknown homebrewed salt, with unknown amounts of contmainations or toxicity ingested on empty stomach. This is what's known in scientific circles as "Very Very VERY Stupid".

2. Contemplate my decisions in life. Was my old girlfriend right all along? Am I a complete and utter idiot? Well I might be, but I'm not dead yet.

3. 8:45. Nothing more. Just the grey sludge of self doubt and frustration of failure.

4. 8:55 You know, this thing my girlfriend is telling me about her day sounds really damn interesting! We need to discuss this further, Theres lots of angles to it.

5. 9 PM about. You know, just about everything I think about is really really interesting and should be brougth up for discussion really. But I think I should probably shut up for a while, however incruciating it is.

6. 9.20. Ok. Now the goddamn FOOTBALL on TV is interesting. I AM OFFICIALLY HIGH AS FUCK, Sports are for retards and people who writes with caps. Better fake a yawn and a stomach ache and claim a need to sleep alone tonight. Cause there won't be any sleep tonight unless under full anesthesia. Beacause the hairs on the back of my neck stand up now.

7. 9.30 PM ---> 8 Am and beyond.
Small hairs standing up and pleasant chills running through my body continues for like 1-2 hours.
I wrote three articles, two porn novels, chattted with people on certain social forum until they bannned me, I catalogued everything on my hard drive really neatly. REALLY. NEATLY.
Wrote another skeleton article. Found a good porn site. The end.

This is probably the most potent speed i have ever consumed. 24 hours and I'm still jacked. I'm starting to get to the point where some diazepams can actually help me sleep, maybe, but if I'd taken those yesterday I'd probably only get really bad balance and fall over stuff- while doing all of the above.


TLDR: I made a-oil through teh NaBH4/copper route and thought it was shit. Tried acidfying it, got jelly-like solution. Jelly became salt in vacuum buchner. Salt smells sickeningly flowery. Some idiot ingested it to try it and is now writing very long messages 24 hours later. Very potent speed!
BBIT WHY DOES IT SMELL LIKE GODDAMN FLOWERS?

Or not flowers really. Like some really baaaad chemist from some eastern European country that always has singers that looks like wannabe porn actresses attend the Eurovision tried making a smell for a toilet cleaner that he'd call "Flowery". That kind of flowery. The bad kind.

 

[MadHatter]

Oh, one more thing: if you have a speed like this, how much cleaning should it go through to be deemed somewhat safe for I.V use? (I mean except for the normal side effects like loosing your teeth with your mind and relations, and end up performing fellatio for money on street corners)
And what kind of cleanings?

 

[mithyl2]

Very happy for you that you finally got some speed.

Wouldn't a standard acetone wash with a buchner funnel be sufficient?

also maybe get it energy tested

 

[MadHatter]

Yes, of course you're right. I did an acetone wash on a minor part of the (terrible) yield and the floral smell was actually essentially gone just by that. God they must have been lazy and sloppy in the 90's.
Also, what do you mean with "energy tested"?

 

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