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

[Curiousonion]

It would affect the yield, sodium borohydride creates an exothermic reaction and that's how it works.
You could try to keep it steady at around 60c while you add the p2np but it could be quite hard.

 

[ElementalEnigma]

I was thinking maybe dissolving the starting material in IPA and slowly drip it into the reaction vessel using a SEP funnel. You recon that would affect it negatively in any way?

 

[WinterDust]

Hi,

Did my second attempt today, and it went much smoother this time.



As you can see in the picture,

To the left you have the "waterlayer" after extraction with NaOH 25%, and to the right you have the amphetamine-oil, freebase, a-oil, what ever you want to call it.

In the waterlyer flask you can see about 5ml of A-oil that I could not extract, I mixed the waterlayer with IPA and extracted the ipa layer, unfortunetly my home made distiller did not work, too many joints to grease and to much hustle, in my opinion it's not worth the extra effort for a few extra ml.

I will need to invest in a rotovap later.

The amphetamine-oil was cleaned three times through buchner funnel and clean filters each time.

Let me know what you think.

Best Regards

 

[ElementalEnigma]

You can add some non polar solvent to aid extraction.

 

[WinterDust]

Hard question to answer, since I built my own cooling system.

 

[ElementalEnigma]

What did you use for a cooling system?

 

[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?

 

[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?

 

[Pervitin]

O.K. splitt off the destilation water, or for what the dean stark? I want to buy a small membrane laboratory vacuum pump with 5.5 - 6l pumping energy. Is this enough for a 10l vessel? Also have a intense condenser.

 

[UWe9o12jkied91d]

Dean stark is so that you can connect vacuum pump to the top of the vertical condenser and have your condensate drop down to be collected,With a normal distillation condenser that sits horizontally you cannot connect vacuum this way since you will flood your vacuum line.
You can try the pump I guess won’t hurt

 

[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"

 

[ElementalEnigma]

What did you use for a cooling system?

 

[G.Patton]

Ice water bath or cold water flow jacket for reactor batch.

 

[ElementalEnigma]

You guys have any issues using DI water instead of dH2O?

 

[WinterDust]

You can use normal tapwater if it's clean.

Works perfectly.

Saves alot of money also.

 

[ElementalEnigma]

Hey guys need your help asap is there something you can substitute the CuCl2 with something that's easily accessible?

 

[UWe9o12jkied91d]

CuCl2 is as accesible as it gets

 

[ElementalEnigma]

WHere can you get it on short notice? Is there any domestic use for it? don't really have time to wait for parcel.

 

[UWe9o12jkied91d]

You can make it short notice with copper sulphate by electrolysis with a lead electrode.

 

[Pervitin]

Hello, I read some time now in this forum?thread and want everyone in this topic to ask what point of the synthesis is for him the most difficult/ important and on witch details everyone should pay attention to?

And in the video is no exactly shown, Is it better to use a reflux condenser for the synthesis?

 

[WinterDust]

No part is difficult in this synthesis, it is just about being careful so there won't be any accidents.

I have had them and wrote about them here in the thread for other people to not do the same thing.

Yes, you need to use reflux condenser.

 

[ElementalEnigma]

Exactly! You can skip reflux but you loose quality and I believe some for of side products form. Anyone find a variant with more euphoric effect form?

 

[Pervitin]

I read about problems with storing the pure freebase, over a couple of time its react. What have to be done to store it propably? Do I need an exsikkator?

 

[WinterDust]

For what reason do you need to store it?

Yes, is degenerates over time. The ideal storage would be in a vacuumcontainer stored inside a fridge.

 

[UWe9o12jkied91d]

Just store the stable sulphate salt and base it when needed