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

[WinterDust]

Hi,

So this is what I did today, I vacuum filtrated my amphetamineoil today from this Jelly compound that had formed and I took a picture of it, look below.



First notice, this is not ice from water, it does not melt and it is honestly just like crystalized Jelly.

Second, from a batch of 15L of amphetamineoil, this compound had a volume of 2,5L

Third, when I did an attempt to crystalize my amphetamine oil, it went much smoother and it came out practically white as snow.

So, I am currently doing a test to see what this can be, I poured a glas of NaoH 25% solvent into a glass and put it in the frezzer, and I'm going to see in the morning if it has turned into this Jelly form or not.

Best Regards

 

[Mystery_chemistry]

this happened to me twice. I have a theory: it could be polymers. which may have been caused by too high a temperature during the reaction. what do you think

my theory comes from the fact that once I had too high a reaction temperature and the second time I evaporated the alcohol for too long and it burned out

 

[Mystery_chemistry]

In my opinion, there are two key moments when this can happen. in the reduction of p2np or in the purification of the free base and evaporation of the alcohol

 

[WinterDust]

Hi,

I would debunk the temperature theory because my temperature is highly controlled and checked every minute with thermometer and digital thermometer.

Evaporated IPA is unlikely, I use a reflux condenser that never goes above 12C so the IPA stays in the batch.

 

[Mystery_chemistry]

impurities may be present in the organic phase. when it evaporates to 90 degrees, nothing like this is formed. however, it was created when I evaporated the alcohol for too long due to low ambient temperature very slow increase in temperature after evaporation of alcohol

 

[WinterDust]

Hi,

So my little test backfired I made a new batch yesterday and I put the whole batch in the freezer, but the whole batch froze.

Note: This time when I put it in the freezer I did not put it in a closed container as I did the last few times. So the difference has been between closed and open container that, open container, the whole batch freezes, but with a closed container only 1/3 freezes. Weird!

My little NaoH 25% experiment did not give any results, it does not freeze at all, so we can rule this compound out from the equation.

So for my next little experiment, I am going to dry the compound using MgSO4 or Na2SO4 then put two batches in the freezer, one in a closed container and the second in an open container.

Best Regards

 

[mithyl2]

cool. let us know what happens!

 

[G.Patton]

We posted new video about synthesis!

 

[WinterDust]

Questions.

Step 9, Why do we dissolve the freebase with acetone?

Which amphetamine type is obtained from this synthesis, is it racemix between d-amph and l-amph?

Best regards

 

[G.Patton]

Hello, It have to be done in order to avoid over acidification of amphetamine. Amphetamine base will be damaged by acid without solvent.
racemic

 

[WinterDust]

Followup question,

Step 9, Can IPA substitute Acetone?

Best Regards

 

[G.Patton]

yes

 

[Mystery_chemistry]

hello, i have one question.

after adding the alkali and collecting the top layer, I wanted to evaporate the excess IPA .. unfortunately it was done in a cold room and it took a very long time ... the greenish solution turned orange-red. I performed an extraction with petroleum ether. I evaporated the ether to 60 degrees, then added a 25% naoh solution to raise the pH. The pH in petroleum ether was on the border of 7-8. after adding alkali it increased to 12-13. two layers were formed. upper orange I collected . I added acetone and added acid ... the paste came out yellowish.

AND NOW MY QUESTION: the reaction was carried out on 1kg of p2np. usually I get about 800 ml of free base from one kg ... this time, because the solution turned red and I extracted it with ether, I got only about 400 ml. extraction was carried out 3x 1l per 5l of red solution ...

why did the solution turn red? too long heating and evaporation has an impact on the formation of additional impurities?

 

[UWe9o12jkied91d]

Yes, heated too much a sol. of freebase will turn red.

 

[G.Patton]

Agree with @UWe9o12jkied91d, you did too long heating exposure on air. Oxygen reacts with amine. It is worth to use rotovap for this purpose.

 

[Mystery_chemistry]

hello , can you replace cucl2 eg sncl2?

 

[TerminusEst]

Love this Synthesis, did it for the first time, works reasonably good with 50 % yield, i think i didn't thoroughly extract the aqueous phase.
Just feels alot better then the reaction via mercury nitrate since even with protective gear that always kinda feels like your poisoning yourself.
Anyhow i have a few questions that i couldn't find the answers to.

1) addition of p2np is really slow due to high heat production, last time i added over multiple hours but is it possible to cool my reaction vessel in a water bath to cool the RM quicker back down ? would help greatly to cut down on time since this step is really the longest.
2) can this reaction be done in a stainless Steel pot ? my glasware is good up to 20 grams p2np but i would like to gradually scale.

 

[WinterDust]

A: Yes, you should in my opinion keep the reactor that you are doing the synthesis in, in a cooled waterbath to have better control of the temperature. I do 400-450g batches and it takes me approx. 45min to add all of the P2nP and keep temperature below 50C.
I would say that you can, but not recommended because of corrosion. Better to just invest in labaratory glassware, it also easy to combine with coolers, and other misc. with a stainlessteel reactor it will be a b**ch to connect everything in my opinion.

Best

 

[MadHatter]

Sorry, this is a late and somehow noobish question, but can CuCl2 be substituted for CuSO4? I can't really see why not, if not the sulphate ions interfere with the reaction in some way.

 

[MadHatter]

Ok, so I did my own research and in the HUGE discussion thread on one of the largest forum for clandestine chemistry this has been tried successfully over and over again. There is some debate as to the yield produced by swapping the two reagents, but it seems like it can swing both ways. CuSO4 is even prefered by some since it tends to produce a less violent reaction upon addition.

I'll have a go with both. Report back.