Syntéza amfetaminu z P2NP pomocí NaBH4/CuCl2 v jednom hrnci (měřítko 1 kg)

[SelfExper1menter]

Dobrý den všem. Pokusil jsem se v malém měřítku vyrobit amfetamin podle tohoto receptu, ale nepodařilo se mi to. Vše se zdálo být v pořádku, po vysušení můj výrobek vypadal jako bílý prášek s nádechem do červena. Pokud by se jednalo o amfetamin sulfát (který jsem se snažil vyrobit), výtěžnost by byla 84 %. Problém je, že to není amfetamin.

Fyziologické účinky
Zkusil jsem 20-30 mg, určitě došlo ke stimulaci, ale také to způsobilo horečku a zřejmě pokles imunity: v obou případech, kdy jsem to bral několik dní po sobě, jsem onemocněl infekcí dýchacích cest (poprvé jsem si myslel, že je to náhoda). Jiný člověk, který ho užíval, nepociťoval žádnou stimulaci od dávky do 90 mg, pouze určité sucho v ústech. Ani jeden z nás nemá žádnou toleranci na stimulanty.

Chemické testování
1 g prášku se zcela rozpustí v 10 ml H2O.
Když jsem k odměřené hmotnosti prášku ve zkumavce přidal přebytečný roztok NaOH, získal jsem přibližně správný objem volné báze páchnoucí po čpavku. Oddělil jsem vrstvu volné báze, vysušil ji CaCl2 a zkusil ji titrovat kyselinou. Výsledkem bylo, že jsem naměřil molární hmotnost freebáze přibližně 171 (a pro amfetamin je to 135). I když moje měření nebyla příliš přesná, rozdíl je stále příliš velký na to, aby se dal vysvětlit pouze chybou měření.

Moje odchylky od postupu
1) Při přidávání P2NP jsem si uvědomil, že to bude trvat hodiny, takže jsem byl netrpělivý a ponořil jsem reakční baňku do vodní lázně o pokojové teplotě. Poté se mi podařilo přidat P2NP téměř najednou a teplota směsi nepřesáhla 40-50 °C.
2) Postupoval jsem podle videa, takže jsem neodpařil IPA a přidal jsem konk. kyselinu sírovou přímo do vrstvy IPA/freebase.
3) Aceton jsem zrovna neměl, takže jsem ho před okyselením nepřidal a přefiltrovanou "amfetamin sulfátovou" pastu jsem promyl IPA.
4) IPA je méně těkavá než aceton, takže jsem musel dát svou sraženinu na několik hodin do trouby, aby se vysušila na konstantní hmotnost. Teplota v sušárně nepřesáhla 80 °C.

Takže hlavní otázka zní, kde se stala chyba? Nepřekvapil by mě nízký výtěžek nebo žádný produkt, ale získat dobrý výtěžek aminu, který není amfetamin?!

 

[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 ?