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

[WinterDust]

Hi, have some questions about the synthesis.

6. 25% water solution of NaOH (8 liters) was added to reaction mixture and the phases were separated.

Q: You ad the NaOH to the synthesis and it splits into two laywers, and you drain the bottom layer and keep the upper layer?

7. The aqueous phase was there after extracted with 8 liters of IPA.

Q: I don't understand this part, after separation from step 6 you ad 8l of IPA and mix it?

8. IPA was evaporated on vacuum to an oil.

Q: Can I use a homemade small distiller to evaporate the IPA? And at what temperature should it be evaporated 60C?

9. The oil was dissolved in two liters of acetone.

Q: I don't understand this part, you ad the acetone to the oil and then start with the sulphuric acid step to get it into the right pH?

Bdst regards

 

[tucoXxX]

hi I am looking for answers to these questions. if you got it, can I see it? I'll go through the thread to see if I can find it.

 

[WinterDust]

I am currently doing batches of 200g of P2nP.

I have quite good cooling method so my temperature never exceeds 47celsius.

It take 1h to add the whole portion of 200g.

Once you add the P2nP the reaction takes a little while to occur the first time, and it starts to foam, during foaming. Don't add more P2nP! Wait until the foam settles and you can see 60% foam and 40% liquid, that is the "soft spot" to add another portion.

 

[Gerald Cotten]

Hey man, can you tell me more about your cooling method? I am very curious.

 

[gcblin]

Can someone explaine this white layer at the bottom i finished adding p2np to nabh4

 

[WinterDust]

Hi,

What do you mean by "Finnished adding P2nP to NaBH4"?

You ad P2nP to the reaction mixed with IPA + H2O + NaBH4.

The NaBH4 settles at the bottom of the reaction if you stop stirring it will "rock up".

Best regards

 

[MadHatter]

Yup, like the man said, it's borate crystals. Also, if you leave the rm cooling overnight for some reason, ice-like boric crystals will aggregate at the bottom. Like a small glacier. I got this on a massive scale at my first run and really wondered what i was looking at. Tested, and drew the conclusion it had to be boric crystals.

 

[MadHatter]

after several experiments I can say that any of these reaciotns involving more than 4-5 g:s og P2NP will require overhead stirring. What happens is that when water gets consumed by reduciton nad iPA gets boiled off, the borohhydride starts to reciitate at th ebotto of the flask. Eventually it will sto the agnetic stirrer, and without agitation more will cystllize quickly into a large white solid at the bottom, not doing ny reduction. Temp will go down, H2 evolution stop.
I broke up the solid cake manually and heated the mix to 60, swirling,, running the magnetic stirrer to the max and jabbing any bigger pieces with my glass rod, but they were very difficult to dissolve.
After I managed however, temp started rising again. I also added 10 more g:s of NaBH4 about 10 mins before hte CuCl2, and the reaction upon addition was vicious! I added 15 ml as fast as I could, with some overbubbling as a result. After that, the reaction ran itself at almost 80 degrees without the need for external cooling, In the end, I had o quench the reaction with external cooling to sleep. I then had three layers in the collecting flask; clear upper layer, thick cake of coper oxide and a lower, brownish red lig´quid layer, where the reaction was still ongoing. Bubbles were shooting uo through the oxide layer konstantly, and they still werein the morning. Now every liquid part had gone transparent though. The third layer now consists of a growing layer of borate crystals,.Coolong the flask seemed to worsen the situation, and tomorrow I will acidify the contents with HCl to pH2 and distill off all the IPA:. I'll then basify it to H10, and steam distill the freebase. Sep funnel, then acetone, tehn phosphoric acid to pH 7.
We'll see whaat I get. '

 

[WinterDust]

Hi MadHatter,

This is not true, I do 450g reactions in a 20l fbf with 8x60 magnetic stirrer and did not once have this problem.

Best regards

 

[MadHatter]

And yet you just said borates build up in the bottom of the flask. If they do so enough, of course they will disturb the stirring?
Overhead stirring it is for me. I already have the setup. Overall, I think vicious agitation is key to the success of this reax. However you choose or can.

 

[WinterDust]

@MadHatter,

Not quite, what I said was that you need to keep stirring during addition of NaBH4 if it STOPS then the NaBH4 will rock up and it will be difficult to get it stirring again, but it is possible.

I do however agree that overheadstirring would be more reliable and better, but in my case it's one component less, and no special two-/three-headed flask is needed.

Best regards

 

[caesare.robot]

swim Granny used to try this method in 100g p2np/2L flask... magnetic stirrer didn't work and then it became different))) working with gloves and hand shaking gave a result of 40g Aoil after water distillation... and that are the good news...
bads are that grannys hands got burned with hot borates in ipa through thick lab gloves! lots of exhaust even via active reflux! be careful!
now granny is on vacation detoxing this method

 

[UWe9o12jkied91d]

Do you look like michael jackson now?

 

[caesare.robot]

mercury, Freddy...(ll)

lol

 

[WinterDust]

Hi,

Long time since I posted some progress here.

So I did my first 1kg batch today, and the result is ≈10l of mixed freebase/ipa/water.

So I will try to do my first purified amphetamineoil with this.

First step now is to use dry agent Na2SO4 to remove the excess water.

Second step will be to evaporate IPA using vacuum distillation

Third step will be to ad distilled water 1:1 ratio and vacuum steam distill of any left impurities.

I will keep you posted of my progress the upcoming days.

Here's a picture from todays reaction

 

[blackburn]

Nice, should you use rotary evaporator to get your amphetamineoil?

interesting to know how long it takes approx to distill of the ipa

 

[WinterDust]

@Sweswe

No, I don't use rotovap, normal distillation kit with vacuum and magnetic stirrer.

Once the water is dried out I will post result from the whole reaction and approx. time for evaporation.

Best regards

 

[MadHatter]

Beautiful! But ... if you distill off the IPA you will effectively steam distill off your product with it, right? So you'll need to acidify your IPA/product mix before distillation. That way your product will not be volatile. Don't do what I did once though: under certain conditions acidifying with strong HCl (>5-6%) will create a reaction that is exothermic and converts your product to P2P somehow. I ruined an entire 20 g batch this way, ended up with just a flowery, yellow oil at the last steps, really irritating. Use acetic acid instead, wekened to 10% or so. Then, after the IPA has been distilled off and the remaining rm has cooled, it's basified again to pH10. Then the freebase can be steam distilled. No point in using vacuum in this step though.

 

[tucoXxX]

Third step will be to add distilled water 1:1 ratio and vacuum steam distillation of any remaining impurities.
---- if you do this, doesn't the pleasant smell of the oil disappear? (it has a classic scent)

 

[WinterDust]

@tucoXxX

I need to distill the amphetamineoil from impurities to be able to produce a quality product.

And, pleasent smell? It's amphetamineoil not a new whiskey brand for rednecks to drink.

Jokes a side.

Best regards

 

[MadHatter]

The "pleasant smell" is the flowery smell of P2NP reduced to P2P, in other words: impurities. Many users connect this smell with amphetamine, even extra strong amphetamine, but it's really just impure leftovers of side reactions. Redspect to ImOut for doing a proper job!

 

[gcblin]

After 4 sucsesfull synthesis i encountered a problem amph salt allways came out withe like chalk but this time after drying it had a yellow hue, also when acidifying at 7ph the whole mixture became slightly red but after a few more drops of acid to reach 6ph it again became white instantly.

Question on drying at what temperature does amph salt desintigrate i was drying it in the oven at 90c it burned at the edges.

Can incorrect drying create a yellow hue on amp salt? Does burned amph create any toxins?

 

[MadHatter]

I dont remember the exact melting point of amph sulfate now, but it's well above 90 C, I think its closer to or slightly above 200 C, and just below the degradation temp.
Yellow hue might also be because of P2P impurity, does your yellow salt also smell flowery? Acetone wash or recryst will remove that.

 

[aa1178251182]

Ask you, amphetamine phosphate, how should I take it? What is the most convenient way to use it?

 

[aa1178251182]

No idea what went wrong, no testing equipment. The resulting amphetamine phosphate has no effect at all.

 

[G.Patton]

Check its melting point. Also, how much have you sniffed?

 

[aa1178251182]

I don't know how to use it, I took about 0.5g, snorted a little, it didn't work at all.

 

[aa1178251182]

I don't know how to use it. I swallowed 0.5g and inhaled a bit through my nose, nothing works

 

[aa1178251182]

thank you very much

 

[Hank Schrader]

Make sure you have phenylnitropropene and not nitrostyrene. Perhaps you were sold an analogue, and you received phenylethylamine.

 

[G.Patton]

Hello. Nitromethane and nitroethane have different b.p. 101 and 114 °C respectively. You can check it and carry out fractional distillation. Take it into account that these substances quite toxic and explosive. So far as nitrostyrene and P2NP concerned, just use precise melting point apparatus. It is better to compare known pure P2NP with synthesized new P2NP in one apparatus to check difference. Also, carry out several measurements in order to exclude errors. Count average mp for each sample.

 

[diogenes]

Thank you Patton. I don`t have any suspicion that my nitroethane is not pure, but having read some comments, I thought it would be better to check, so I will start with the boiling point of my nitro and if it boils over 110C then I will rest assured. It is good to know what to do and check anyway, before putting in a lot of work and finding that the end-product is ineffective .

 

[chicaloca]

I have the same problem. I do the reaction and work up but I don't think the salt is amphetamine or if it is so it's a very very poor quality! What I should try to do for improving?