Sintesi di anfetamina one-pot da P2NP con NaBH4/CuCl2 (scala 1 kg)

[William D.]

La reazione con la boroidruro di sodio può andare fuori controllo se non si monitora la temperatura. Inoltre, i composti di rame in piccola quantità possono interferire con la purificazione del prodotto finale.

 

[Johnny Ringo]

Kann man die kupferverbindungen verhinden und ist das produkt(base) geeignet paste herzustellen wenn man es nicht mit aceton wäscht und nur schwefelsäure hinzu fügt?

 

[Johnny Ringo]

Und wie kann man es am besten beheizen, da die kontaktfläche bei rundkolben schlecht hitze absorbiert und es sehr lange dauert wenn man versucht den kolben direkt zu beheizen.

 

[Sasha89]

Cosa si usa per il riscaldamento esterno per mantenere la temperatura a 80 °C per 30 minuti?

 

[GDC]

Piatto di alimentazione per cani in metallo con acqua.

 

[Johnny Ringo]

Bin auf das problem gestoßen,dass das wasser verdampft ist bevor es 80grad erreicht hat könnte ich es mit öl erhitzen?

 

[SelfExper1menter]

Salve a tutti. Ho provato a fare dell'anfetamina con questa ricetta su piccola scala, ma non ci sono riuscito. Sembrava tutto a posto, dopo l'essiccazione il mio prodotto si presentava come una polvere bianca con una punta di rossore. Se si trattasse di anfetamina solfato (che stavo cercando di produrre), la resa sarebbe dell'84%. Il problema è che non si tratta di anfetamina.

Effetti fisiologici
Ho provato 20-30 mg, c'è stata sicuramente una stimolazione, ma ha anche causato febbre e, apparentemente, un calo delle difese immunitarie: entrambe le volte che l'ho presa per diversi giorni di seguito, mi sono ammalato di infezioni respiratorie (la prima volta ho pensato che fosse una coincidenza). Un'altra persona che l'ha preso non ha avvertito alcuno stimolo fino a 90 mg, ma solo un po' di secchezza della bocca. Nessuno dei due ha una tolleranza agli stimolanti.

Test chimici
1 g di polvere si scioglie completamente in 10 ml di H2O.
Quando ho aggiunto un eccesso di soluzione di NaOH a una massa misurata di polvere in una provetta, ho ottenuto un volume approssimativo di base libera che odorava di ammoniaca. Ho separato lo strato di freebase, l'ho asciugato con CaCl2 e ho provato a titolarlo con un acido. Come risultato, ho misurato la massa molare della freebase a circa 171 (mentre per l'anfetamina è 135). Anche se le mie misurazioni non erano molto precise, la differenza è comunque troppo grande per essere spiegata solo da errori di misurazione.

Le mie deviazioni dalla procedura
1) Quando ho aggiunto il P2NP, mi sono reso conto che ci sarebbero volute ore, quindi mi sono spazientito e ho immerso la beuta di reazione in un bagno d'acqua a temperatura ambiente. In seguito ho potuto aggiungere il P2NP quasi tutto in una volta e la temperatura della miscela non ha superato i 40-50 °С.
2) Seguendo il video, non ho fatto evaporare l'IPA e ho aggiunto direttamente acido solforico conc. allo strato di IPA/freebase.
3) Non avevo acetone al momento, quindi non l'ho aggiunto prima di acidificare e ho lavato la pasta filtrata di "solfato di anfetamina" con IPA.
4) L'IPA è meno volatile dell'acetone, quindi ho dovuto mettere il mio precipitato in un forno per diverse ore per farlo asciugare a peso costante. La temperatura del forno non ha superato gli 80° C.

Quindi, la domanda principale è: dove è andato storto? Non mi sorprenderebbe una bassa resa o l'assenza di prodotto, ma ottenere una buona resa di un'ammina che non sia anfetamina?!

 

[OneTensionSkyRed]

That's what I was thinking. This reaction produces N-OH-amphetamine instead of pure amine. People can clearly tell the difference between their physiological activity.

 

[pekonias]

I don't anderstand what is happening? I used 300g NaBH4 2.07 L IPA, 1.03 L dH2O, 173g P2Np 22g CuCl.2H2O and everything went well - reaction over and I add 0.4 L 25% NaOH sol. to get (pH 13.5) separate layers but... there's wery little separation. The aq. layer was only 0.3L so now I have 2.2 L organic layer, more than starting IPA + H2O (2.1 L). So does organic layer now contains NaOH? The pH after reaction was ~12 and there was no layer separation so I added the 0.4 L NaOH sol. What should I do now? Add more NaOH sol. and vacuum distill? Maybe acidify to pH <=3 and distill. Please advice guys.

 

[pekonias]

Obviously I can't count, actually got correct volume for the organic part and also extracted the sludge with 0.3L IPA. It's very confusing when told to add NaOH to pH 12 when it's already at that after reaction. Also aq. part seems to small but it's mostly in the black mud. Going to go ahead with water aspirator vacuum distilling off the IPA and hopefully not lose all product like last time. I think got too hot 80C with -28" Hg vacuum last time. Maybe report how it went tomorrow if has any luck.

 

[OneTensionSkyRed]

You need to add more NaOH in dry form or at least concentrated NaOH solution if you don't want to heat RM from dry NaOH to separate IPA layer. The densities are similar and that prevents IPA from salting out. Have you destroyed borate adducts afther the reaction?

 

[two777]

what is the optimal temperature for a-oil, before you start the extraction/ crystallization process using sulfuric acid? Usually im working with room temperature oil, and adding acid gradually, by not extending temperatures above 40c.

 

[GhostChemist]

this is right

 

[pekonias]

Follow up to my previous post, copule observations made during the process I think are important to share. This was really my very first success at this. From 173g P2NP I got ~130ml clear oil. What I wanna say is that now, compared to the previous experiment, was very different at the step when CuCl added. Previously added it dropwise and the temperature didn't increase at all, no storm in flask and only gave test subjects a runny nose. Now had twice as much and better quality P2NP. Also 10% of the NaBH4 was added later, after most P2NP had been added but it don't seem make no difference. So the CuCl was added added in 3 bursts of 10ml each and very violent reaction was observed (~1/4 CuCl soln. was left unadded). After each 10ml addition the reaction almost came out of the flask but not quite and the temperature increased dramatically. The Rm was 3.1 L in 5 L RBF. Temp reached 78C after third addition and the surface / foam level stayed really high for a minute and the reflux from the two ball condensers poured down IPA/H2O like hell. Unreal sight but it happened and I think the reflux prevented temp. going > 78C. So I much rather want the violent reaction then I know something is really cooking and reacting. The organic layer was condensed in -26.25" Hg vacuum BP 37-38C. Vacuum dist. stopped when 1.8 / 2.2 L liquid was removed (BP. was 41.8C at end). Then steam distilled. First 100ml of distillate thought to be water and almost thrown away! It's A-Oil! Thinking drying some of it by mixing 50ml Oil with 300ml? dry IPA and giving it 20g silica gel and let sit overnight. How much H2O should the vacuum distilled IPA contain? Would be nice to re-use it. I measured its density to be ~0.8g/ml which is that of IPA (0.786g/ml) within the measurement accuracy?

 

[OneTensionSkyRed]

DO NOT dry it with silica gel or molecular sieves. They are acidic and should not be used for drying amines.

 

[keras]

So to cook 1kg of amph would cost more than to make 1kg 3cmc?
Becausd borohydride I see costly in poland , also p2np add up. While 3cmc is one main precursor.
And how these guys sell amp paste for less than 1k per kg. Where profit comes from ?

 

[dobrytowar55]

So then i Ask for most beacuse i knows on netherland production cost is between 300-600euro. How ? I dont mnie but meaby someone tell me herę

 

[dobrytowar55]

Hi. Can someone tell me what the cost of ingredients and equipment for producing 1kg is? I would be grateful if someone could tell me if it is enough to scaling up everything to get a larger amout or does that cause any discrepancies? Also can someone tell me what is the CAS of this final product?

 

[OneTensionSkyRed]

It would be really REALLY great if someone could run a TLC analysis of the products from this reaction. I've read that NaBH4/Cu reduction mainly produces N-hydroxylamines instead of amines for alpha-alkyl nitrostyrenes. Because of similar melting points for their salts and similar boiling points, the only way to separate and identify N-OH-amphetamine is by chromatography. The N-OH product is also active as a stimulant but it is different to amphetamine. I wonder if this is really true.

 

[GhostChemist]

what source reports this information?
all compounds tested with qualitative and quantitative analysis
N-OH group can be formed as an intermediate compound if the experiment is not carried out correctly

 

[OrgUnikum]

No. N-Hydroxylamphetamine is not stable in ph >7 it would go instantly to the Oxime and then back to the carbonyl say P2P.

 

[rampage]

is Copper (II) Chloride Dihydrate ok to use or does it have to be Copper (II) Chloride?

 

[GhostChemist]

In this synth dihydrate is used

 

[gmanaus]

I used copper sulfate and dried it till gray and it worked just fine

 

[GhostChemist]

If it is really works, then this is a good experience