Sinteza amfetaminei la o singură oală din P2NP cu NaBH4/CuCl2 (la scara de 1 kg)

[SelfExper1menter]

Bună ziua tuturor. Am încercat să fac niște amfetamină folosind această rețetă la scară mică, dar nu am reușit. Totul părea în regulă, după uscare produsul meu arăta ca o pulbere albă cu o nuanță de roșeață. Dacă ar fi fost sulfat de amfetamină (pe care am încercat să îl fac), randamentul ar fi fost de 84%. Problema este că nu este amfetamină.

Efecte fiziologice
Am încercat 20-30 mg, a existat cu siguranță stimulare, dar, de asemenea, a provocat febră și, aparent, o scădere a imunității: de ambele ori când am luat-o timp de mai multe zile la rând, m-am îmbolnăvit de infecții respiratorii (prima dată am crezut că a fost o coincidență). O altă persoană care a luat-o nu a simțit nicio stimulare de până la 90 mg, doar o oarecare uscăciune a gurii. Niciunul dintre noi nu are toleranță la stimulente.

Teste chimice
1 g de pulbere se dizolvă complet în 10 ml H2O.
Când am adăugat un exces de soluție de NaOH la o masă măsurată de pulbere într-o eprubetă, am obținut un volum aproximativ corect de freebase cu miros de amoniac. Am separat stratul de freebase, l-am uscat cu CaCl2 și am încercat să îl titrez cu acid. Ca rezultat, am măsurat masa molară a freebase-ului la aproximativ 171 (iar pentru amfetamină este de 135). Deși măsurătorile mele nu au fost foarte precise, diferența este totuși prea mare pentru a putea fi explicată doar prin erori de măsurare.

Abaterile mele de la procedură
1) Când am adăugat P2NP, mi-am dat seama că va dura ore întregi, așa că am devenit nerăbdător și am scufundat balonul de reacție într-o baie de apă la temperatura camerei. După aceea am putut adăuga P2NP aproape dintr-o dată, iar temperatura amestecului nu a depășit 40-50 °С.
2) Am urmărit videoclipul, așa că nu am evaporat IPA și am adăugat acid sulfuric conc. direct în stratul IPA/freebase.
3) Nu aveam acetonă pe moment, așa că nu am adăugat-o înainte de acidificare și am spălat pasta de "sulfat de amfetamină" filtrată cu IPA.
4) IPA este mai puțin volatilă decât acetona, așa că a trebuit să pun precipitatul meu într-un cuptor timp de câteva ore pentru a-l usca la o greutate constantă. Temperatura din cuptor nu a depășit 80 °С.

Așadar, marea întrebare este, unde a mers prost? Nu m-ar surprinde un randament scăzut sau niciun produs, dar obținerea unui randament bun al unei amine care nu este amfetamină?!

 

[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

 

[chemdogpal]

at what temperature does amphetamine start to evaporate ?