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

[Montecristo]

Here was what i did on a smaller scale;
1. Solution IPA/H2O 2:1 ((IPA 800ml,H2O 400ml)(1200ml)) was added a 2000ml flask.
2. NaBH4 (116 g) was added at once and stirring was started.
3. P2NP (67 g) was added in small portions, so that the temperature of the mixture did not exceed 60 *С.
4. CuCl2 (7 g) in water (13 ml) was added slow dropwise, so that the temperature of the mixture did not exceed 80 *С.
5. Thereafter, reaction was refluxed at 80 °C for 30 minutes using external heating.
6. Solution is decanted and filtered from reaction waste and put into a seperatory funnel.
7. 25% water solution of NaOH (533ml) was added to reaction mixture and the phases were separated.
8. Drain the bottom layer into a large beaker and collect the top organic layer.
9. The aqueous phase was then put into the seperatory funnel and extracted with 500ml of IPA.
10.IPA was evaporated by 3/4, half milky freebase and half IPA.
11.The IPA and freebase was dissolved in 130ml of acetone.
12.orthophosphoric acid dripped to pH - 6 (with constant stirring).
13.The mixture was put in the freezer for 12 hours.
14.After crystallisation the suspension was filtered and washed with dry cold acetone, until acetone is clean.
15.Acetone from washing and the ipa/acetone mix is placed back into freezer for further precipitation.
16.Process repeated until no more precipitate to yield 60-70% high quality amphetamine, as the mix gets more acetone in it you may need to drip some more acid to bring it down, but not too much as acetone is ph7.

Here is a photo of some of the dried paste rocks , the rest is dry powder to be mixed, as it is too strong for me and my friends.
I may update the recipe and do a write up for the small scale home chemist, there are lots of ways this could be better.

 

[flyhigh]

this is no meth , can you write from here on how to make it to crystal meth

 

[Amin. M]

What method do you use to convert this white paste into crystal
d-methamphetamine?

 

[Curiousonion]

Isn't sodium borohydride expensive?
And at 3 kilos to produce 1 liter of amphetamine oil the cost would be a bit too much for it to be attractive.

 

[flyhigh]

good question.

 

[antrax]

Did you finally synthesize amphetamine sulfate (speed) following this route?

 

[Curiousonion]

Hi

Thanks yes I saw that. I also found a supplier in spain for p2np for around 215€ per kilo. Even if I synthesis it myself at that price it's cheaper to just buy it pre-made

 

[antrax]

Could you give me the contact of said Spanish P2NP CHEMICAL supplier?

 

[InLikeFlynn]

Just did my first synthesis using this method with a 45% yield on 5g of P2NP.

this was my absolute first time so I’m sure I made some mistakes along the way, but I just wanted some experience. Ended up having a very fun time. Totally found my new hobby here. Can’t wait to get into some more experiments and improving on my techniques.

much love to those who run this site, I wouldn’t have been able to do this without the visual aids, helped fill in a big gap in my knowledge just watching the videos.

 

[mithyl2]

awesome!

sorry to keep on about this, but what did you do for your air filtration to deal with the hydrogen gas?

 

[InLikeFlynn]

I had my set up right by the opening of a doorway to the outside and a larger box fan pulling air from my work area out the door way.

Probably not the most effective or airtight way (like a fume hood) but I did see the vapor fumes from my reflux condenser being sucked through my fan and into the outside air. For smaller experiments, it does seem to be effective though.
Another idea I had before this was to put some sort of hose adaptor on the top of my reflux condenser and attach a vent hose to the outside that way.

I will be building a fume hood in the coming months as I’d like to have a more proper setup and I would just recommend building one as well if you’re at all paranoid about this.

 

[mithyl2]

yes i was going to use a hose leading from my flask to the outside of a window with a fan blowing behind it.

what type of motor does your box fan use?

to begin with i'll be doing a synth using 10g p2np. how much hdydrogen gas do you estimate is produced with a synthesis of this size?

 

[mitea]

I did the first sample, and I have some questions.

- At 75% of the P2NP addition, the color of the solution changed to slight brown. Is this normal, or my P2NP is contamintated and need to be crystallized before?

- To make the P2NP addition faster, I added the flask to a cool water bath. Does this make a difference in the final product quality or quantity?

- I forgot to add acetone before adding H2SO4. Is this a problem? I added acetone before I added 1/3 of the H2SO4 quantity (also I had 1/2 of the required acetone quantity).

- I don't had acces to a watter source to cool the condenser. The IPA evaporated sligtly during the reaction. Can this lower yield?

 

[Gordon Ramsay]

Do you have a picture? It should not be normal.

You can carry out a melting point determination to estimate the quality of your P2NP.
A recrystalization would be recommended.

Another reason could be impurities inside of your glass, like copper residues from previous reactions?
External cooling is required for this synthesis if you are looking to speed up the addition of P2NP.
It is important to not cross the target temperature during the addition of P2NP and not cool down the reaction too much because it will stop if you do so.

Exceeding the temperatur would influence your product quality or yield more I would assume.

My sweet spot is around the 55 - 58 °C during the addition of P2NP.
Acetone will help during the vacuum filtration happening after the amphetamine salts have formed. It will clean the product but forming the salts without Acetone would also work.
You can build your own water source with a 15EUR aquarium pump from amazon, a bucket and a fridge.
Alternatively there are industrial water coolers that you could purchase for around 100EUR.

It will be helpful to not have too much IPA evaporating at this stage but it is not needed for the chemical reaction happening

 

[Xiao hua]

hello everyone. How can make amphetamine crystals

 

[mithyl2]

what are the main reasons for not getting a full yield with this synthesis?

 

[InLikeFlynn]

On a small scale you need to let the NaBH4/P2NP addition reflux at 60C for a good 30/45 min after completion of the addition. I’ve read this results in incomplete reduction.

at larger scales such as the OP, it’s not a big deal since you have so much P2NP to add it takes forever and the step is unnecessary.

other than that what issues are you having?

 

[mithyl2]

yes, it only took me about 2 hours to add all of the p2np because i only used about 5 grams of it and i'm not sure i let it stir for long afterwards.

there were several problems with the first synth like not keeping the temperature maintained at 80c for the 30 minutes needed, or stirring the copper until it suddenly became thick (which was wierd) instead of just swirling it a bit like in the video, and raising the temp by a lot when i added the copper solution...

i'll try again with these problems fixed. if there might be anything else you can think of that might be a common issue please let me know

 

[InLikeFlynn]

This thread on Reddit has a ton of great info on the 5g scale. It was actually made in reference to this thread here in BB. I basically followed it word for word and have been successful.

https://www.reddit(.)com/r/TheeHive/comments/12hcbrr/complete_nabh4_copper_salt_reduction_n00b/

 

[mithyl2]

thanks for that!

did you do an a/b extraction? i tried, but but failed because i couldn't get the amphetamine to crash out at the last step. i was using only 2g of product, so absolutely tiny quantities.

 

[InLikeFlynn]

I tried to but when I went to add acetone to the freebase/DCM extract that I pulled, it would also not crash out when I attempted to salt it. It also created an emulsion layer and separated the DCM and acetone.

I suspect I should have evaporated the DCM before adding acetone to the freebase. But I haven’t had a chance to get to that just yet.

 

[mithyl2]

ok.

i used xylene as that was the next best (and available) solvent.

what quantity of amphetamine did you use?

 

[w2x3f5]

Thanks mithyl2 for your experience first of all.
In my opinion, for this reaction it is possible to make additions that may increase the yield and purity of the substance:
1) Use a sufficient amount of borohydride to restore the double bond, that is, from nitropropene to nitropropane.
2) Next, introduce acetic acid into the reaction in excess, sufficient to bind the free base and side reactions to form sodium acetate and other substances.
3) It is advisable to prepare the copper catalyst separately from copper chloride, sodium borohydride in cold water and wash it with water to remove salts. Or introduce the copper salt into the reaction before adding acetic acid, but the catalyst will be of lower quality.
4) Introduce sodium borohydride or another, cheaper source of hydrogen into the reaction in small portions. At this stage we reduce the nitro group, for this reason the acid will mix the equilibrium of the reaction to the final amine product.

 

[mithyl2]

in reference to your first point, is the prescribed amount of borohydride in the guide already sufficient?

how much acetic acid should be used reletive to the amount of p2np?

 

[mithyl2]

in the video novator says that around half of the 26.25g CuCl2 solution will be enough to 'cease' the black copper oxide formation.

does he actually use all of the CuCl2 solution, or only half of it?

(the last synth i did i added the CuCl2 solution in an unmeasured amount until the black copper oxide forms at the bottom of the reaction mix. i have yet to determine the quality and yield of the final product).

 

[Gordon Ramsay]

I think it was not fully stated if 100% or 50% was used int he video. I think maybe 100% but it was highlighted that it might be enough to stop after 50% of the solution.
You will learn to see when the point has been reached to stop according to how your RM behaves. Yet I use almost most if not just all of it
Copper residues should not be left inside of the final product anyway

 

[mithyl2]

i'll be using my mantle next time because of this.

its a ceramic hotplate. at first it was set to 83C but the solution wouldn't go past 60C. and it took a long time to get there from about 50C. then i turned the hotplate to 100C, nothing changed with the solution, then set the hotplate to 120C, and still nothing changed. it's happened before with other synths.

and before heating it i wrapped the flask in foil.

 

[Gordon Ramsay]

Good, a heating mantle will help.

It is important to wrap the flask and also the lower part right above the heating plate. It can also be outside vactors like a fan or something else blowing cold air that prevent the flask from heating up to 80 °C

 

[InLikeFlynn]

Whatever you do, do it on a mg or gram scale first just so you can see what’s going on. That’s a lot of product to waste if you mess up somewhere.

 

[mithyl2]

I always appreciate tips from real experience. I haven't tried dry IPA yet

what is your source of p2np?

 

[InLikeFlynn]

Found it on eBay. Currently in the process of teaching myself how to make it.