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

Mystery_chemistry

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20-40 degrees is optimal ... come, in my opinion, it is better to observe how the reaction behaves and not to hold some temperature rigidly ...

these regulations, which can be found on the Internet, are more illustrative to approach them ... only practice will lead to the appropriate results ...
 

KokosDreams

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@DocX @Mystery_chemistry @G.Patton

While doing this in a 20L flask, would you recommend manual cooling with an ice bath same as shown in the Al/Hg route video tutorial?

Also, as the P2NP shouldn't be added at once, what should be the maximum time frame where the whole amount was added?
 

Mystery_chemistry

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yes, throw the butt into the ice and start adding p2np ... the first accusations will be the most buzzing ... when the bombs appear all over the surface you will be able to start adding p2np faster ... practice and observation will learn how quickly and when you can add another portion
 

KokosDreams

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Interesting! Let's say I'd use 1000g P2NP, in how small portions would you split it?

Also, what do you mean with ''bombs'', do you mean bubbles?
 

WinterDust

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Thank you for answering, this will definetly help me out and make it alot easier for me now.
 

WinterDust

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My man, you really need to start cooking yourself soon :)..
 

WinterDust

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Hi,

So I did my second attempt today, and it went very well, I will give a full update soon with pictures of the whole procedure.

But I have one question that I think I missed.



On step 6 I added the NaOH 25% durring stirring, and the layers were separated just like the description, my question is.

The yellow liquid that I have is the freebase (a-oil) and the bottom layer is the aqeuous layer and it is the layer that I mix with the IPA in step 7 then vacuum and later mix with my freebase.

Am I correct?

Best Regards
 
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G.Patton

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You'll understand during reaction. You have to add P2NP and maintain temperature below 60 deg C. It is the most significative parameter.

Hello, good job! Actually you are almost correct. You'll add IPA into water layer in order to extract remains of amphetamine free base from it. Then, separate layers (you need organic one), evaporate solvent and get amph free base oil. Next, you can combine layers and continue salt formation.
 

KokosDreams

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Haha I knoow man, I got the precursors and most lab equipment ready and am only waiting for my 20L flask + Condenser and some other items

My brain is exploding from 6 months learning haha
 

KokosDreams

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Perfect :) Can't wait to try it soon!
 

WinterDust

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Hi,

Just so I understod it correctly.



Like the picture, the waterlayer that is the one that I extract using IPA and then vacuum?

The freebase does not need any more extraction, vacuum? It will only be mixed with the freebase that will be extracted from the waterlayer?

Am I correct?

Because yesterday, I mixed the freebase with sulfuric acid down to pH 6 and it got very thick like whippedcream and crystal white look, it has now been in the freezer for 12h and I am going to vacuum it today and clean it with cold acetone then dry.

Best Regards
 
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Curiousonion

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Once you do the ipa separation you usually vacuum distill the ipa off.
Some people also do a steam distillation of A oil after that to remove every unpleasant smell and make it ultra pure. (but people don't recognize A oil without the stinky smell usually)
 

KokosDreams

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Pretty messy if you think about it tbh, that people would prefer an uncleaned product
 

G.Patton

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Yes, you have to combine free base from water extraction with general part.
 

WinterDust

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Perfect, thank you.

I will do my third attempt tomorrow most likely, but this time I will do the IPA extraction on the waterlayer and on the a-oil. (Full story with pictures will be posted soon enough)

I have another question, the batch that I did yesterday, I stored it in the freezer for 15hours and the mix was just a thick as whippedcream, beautiful white color, it was very hard to vacuum it, took about 2h in total. But I feel that my amphetamine pasta is still too wet, any recommendations on how to dry it carefully?

I currently have it in a plastic foodbox without the lid and left it for two hours in room temperature but it started to turn very light brown, so I currently have it inside the refrigerator instead. Is the refrigerator method sufficient enough for the remaining solvent to evaporate and dry it?

Best Regards
 

Netflix

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Wash him with acetone in next day you get pure powder
 

G.Patton

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You have to wash it by dry (without any % of water) cold acetone to pure white. Then, you can vacuum filter it and place in your foodbox into Vacuum desiccator or another chamber with vacuum.
 

Eidolon-UK

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Some helpful tips from my friend ciphir who was part of the original thread over at the vespiary:

Overhead stirrer is essential, magnetic stirring cannot cope, extremely vigorous stirring is required for the initial part of the reaction when the C=C double bond is broken,
the solution will turn from a yellow to a white colour when this part is over.
The second part, the reduction of the nitro group to amine, goes better with addition of the copper chloride dihydrate (CuCl2.2H2O) solution as fast as possible,
it foams a lot so you can attach the output of an electric vacuum booster pump to the gas port and apply slight positive pressure of air to control the foaming.
Also you can attach a anti-splash straight adapter between the reactor vessel and the condenser assembly to prevent foaming blowing out the top.
Instead of 10 to 20% molar equivalent of copper chloride can also try using you can use a 8% molar equivalent of copper chloride dihydrate and a 8% molar equivalent of copper sulphate pentahydrate, so you are still providing the Cu nanoparticles or NaBH4-Cu complex but with reduced foaming. (Note: 1000g of P2NP means this is a 6.12 mole reaction (1000/163.2 g/mol), so 8% molar equivalent is 0.49 moles of each copper salt.)
Add a saturation amount of common table salt (NaCl) to the water extraction, because it has a higher affinity for water the last load of amine molecules get pushed out of solution and will enter the non-polar layer.

Aside:
I know Ciphir, normally after conversion of the nitro to amine, adds glacial acetic acid until pH=4 to push the amine into the aqueous layer (any fizzing is the quenching of any excess NaBH4, use less next time). Strip off the IPA up to about 97C, then basify to pH=11 with NaOH, now steam distil with a wall paper steamer connected to an inlet into centre of reaction vessel.
Using a 2L sep funnel, collect the water (lower layer) for extraction, save the non-polar layer as this is pure freebase oil of the amine.
Extract aqueous layer 3 x with DCM or another non polar solvent that's immiscible with water, add salt to water layer for final extraction.
Combine organic phase and extracts and distill off NP solvent.
Mix amine oil with 5 parts anhydrous isopropanol (IPA), mix sulphuric acid with 2 parts anhydrous IPA, add until pH=9, then very carefully add until pH=6.7, use buchner funnel to filter amorphous white solid (no crystallisation possible with this amine) vacuum dry solid in funnel.
Check pH of filtrate add more acid if necessary, place in freezer for second crop, repeat process until no more amine sulphate precipitates.
 

diogenes

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Yes, you are right. My bad, thanks for clarifying.
 
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