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

[blackburn]

Hello
after the batch 1kg p2np we have about 10l of diluted ipa/amphetamine, why do we have to add more ipa/acetone to this before we drip in sulfuric acid when there is already enough ipa in it.

when we have pure amphetamine base, we dilute this with amf/ipa 1:2 or 1:3 before adding sulfuric acid...

and is it possible to run the synth with methanol/h20 instead of ipa..

Thanks

 

[G.Patton]

Yes, it is possible. You have to use pure alcohols.

 

[blackburn]

Okey, Thanks

 

[Melv99]

Wondering this myself. Unless I'm mistaken or missing something.. We evap IPA to leave FB then add IPA/Acetone. Can't we go straight to Acetone/Sulfuric since it's already in IPA?

 

[UWe9o12jkied91d]

You can add conc. sulphuric but its always a good idea to dillute it with some acetone.Dropping it in conc. leads to local over-acidification, where regardless of basic medium a portion of your product will be irreversibly destroyed.

 

[Melv99]

In the video it says Acetone is added to the Ipa/base solution. I don't see the Ipa being evaporated off. If it possible to do without the evap step?

 

[G.Patton]

Yes. You can. The difference in crystallization procedure. It will be a little bit longer.

 

[aa1178251182]

After the reaction, the temperature was lowered to room temperature, and I poured 25% sodium hydroxide solution directly into the whole material and stirred. Stand still and divide into take the oily layer, then add 85% phosphoric acid directly to the oily layer. The pH value is adjusted to 6. There is salt precipitation during cooling, but there is no medicinal effect. Is it caused by changing the synthesis steps?

 

[aa1178251182]

The precipitated salt is dried and used without medicinal effect. I couldn't dissolve the precipitated salt with 15% NaOH, the salt settled on the bottom with a small amount of yellow oil on top.

 

[aa1178251182]

steps i changed
1. Add 25% sodium hydroxide directly to the whole material
2. Instead of crystallizing with acetone, directly add 85% phosphoric acid to the upper oil layer. How much does this change affect this route?

 

[G.Patton]

Approximately 0% difference.
@aa1178251182 Why do you repeat same questions. Me and @Hank Schrader have already told you that you have problem with reagent CAS 705-60-2. You have to check its melting point. Instead of this, you ask same questions with hope to hear what? That you can change concentration of alkaline and everything will change? We are chemists, not office managers, you won't get different easy/desirable solution in case problem with reagent (starting material).

 

[blackburn]

Hello guys, what is your best way to dry and how long does it take you? big batches take forever, and butchner funnel is not helping so much...

Some ideas?

Thanks.

 

[WinterDust]

Depends what you use as washing agent and how much of the liquid you manage to vacuum of with buchner funnel.

Acetone / IPA.

Acetone evaporates much faster than IPA thus dries it faster.

After washing my product I vacuum filter it until it stops dripping from the buchner funnel.

So the amphetamine is damp at this stage, I put it in an open container and put it in a freezer for 2 days.

And voila, hard as a rock.

You can basically crush it into powder with your hands.

Remember if you put wet/damp amphetamine in the freezer to dry, open the freezer once or twice a day to let the vapors out.

Freezers unlike fridges are closed loops.

 

[Melv99]

Will any of the Naoh solution make in into the ISO/Amp layer? If so upon salting would Na Sulfate/Nacl also form with the Amp?

The reason I ask if because I recently did this rxn on a small scale and everything worked amazingly amd yield was much more than expected..

For whatever reason I'm second guessing the product obtained (4FA).. I will do another MP test but the initial test melted(or remaining solvent evaporated) and then burned as I would expect nacl would burn. Regeant tests showed no change but that's to be expected with 4Fa.
Haven't tried Robadope yet as I couldn't find any indication.

 

[UWe9o12jkied91d]

do a/b on it, maybe even separate enantiomers if you are at it

 

[Melv99]

Good idea on both.. Makes me wonder if others who aren't experiencing any effects are just consuming a S ton of NaCl and little but of amp.

 

[Pervitin]

When I have to distill of the IPA under vacuum, how high should the temperature be? And what ca I do to optimize the results without drying the acetone?

 

[WinterDust]

Temperature of any compound under vacuum depends on the vacuum pressure.

There are very good charts online for this purpose, google them to get an accurate calculatio set up.

 

[Pervitin]

If I want to volatilize it of, did I have to boil it or only letting it sit for a longer time. When I have to boil it, witch temperature do I have to use?
Secondly, when I want to follow the exact description in the video, how much NaOH do I need? 2 litres of 25% NaOH solution with 500g NaOH for 250g P2NP?

 

[blackburn]

just as imoutalso described it depends on the vacuum pressure, when you distill under vaccum you lover the boiling point you have to try your hand at it.

1500ml water, 500g Naoh, for your 250g P2np batch.

 

[Pervitin]

Thanks, but maybe I don't articulate me right. I found the table in my "organikum" Book too but I thougt it is possible to remove the ipa at normal pressure?

 

[UWe9o12jkied91d]

Possible yes, but you might ruin your product at least partially without an inert atmosphere.But then again maybe it’s perfectly ok, I have only managed to isolate good product under N2.
A vacuum pump is not so expensive, the big AC ones are good(for a while) for stripping solvent, the small 12V chinese ones not so much for this application.
Get a dean stark, bubbles condenser and connect vacuum to the end of condenser, pulling out just enough to not let vapors escape and releasing vacuum to drain by gravity out your trap.

 

[Pervitin]

Yeah I have for this a vacuum receiver and will follow the classic architecture for vacuum distillation apparatus but without a woulfsche flask and only a vacuum gauge direct at the pump.

 

[UWe9o12jkied91d]

nice

 

[ElementalEnigma]

Theoretically speaking is it possible to successfully do this using a 55 galon drum with overhead stirrer as a reactor?

 

[WinterDust]

If you would take the time and read through the thread you would see that this question has been asked multiple times on different scales, and the question remains the same.

Seek, and you shall find.

 

[ElementalEnigma]

Thanks for the tip, While I was scrolling through all the 27 pages I found m any valuable tips along the way. I'm only curious if anyone has tried the technique and how much would it effect the yield by? Comparing to a reactor.
And if there's any tips from anyone who tried it.
Thanks

"Alchemists in search for gold have found many other things of greater value"