Syntéza amfetamínu z P2NP prostredníctvom Al/Hg (video)

[HIGGS BOSSON]

Vo videosyntéze amfetamínu sa používajú činidlá:

• 10 g 1-fenyl-2-nitropropénu (P2NP);
• 100 ml izopropylalkoholu (IPA);
• 50 ml ľadovej kyseliny octovej (AcOH);
• 50 g hydroxidu sodného (NaOH);
• 12 g hliníka (vo forme plátkov fólie pre domácnosť);
• 0,1 g dusičnanu ortuťnatého (II) (Hg(NO3)2);
• 2 ml kyseliny sírovej (H2SO4);
• 50 ml acetónu;
• Destilovaná voda;

Vybavenie a sklenené nádoby:

• Sklenená banka s plochým dnom 2 l;
• Retortový stojan a svorka na upevnenie prístroja (voliteľné);
• spätný chladič;
• lievik;
• Sitový filter (kuchynský filter je vhodný);
• Striekačka alebo Pasteurova pipeta;
• papiere s indikátorompH;
• kadičky (600 ml x2, 2 l, 1 l, 100 ml x2);
• Zdroj vákua;
• laboratórne váhy (vhodné 0,1 - 200 g);
• Odmerné valce s objemom 1000 ml a 100 ml;
• Studený vodný kúpeľ;
• Sklenená tyčinka a špachtľa;
• Oddeľovací lievik 1 l (voliteľný);
• laboratórny teplomer;
• Buchnerova banka a lievik;
• filtračný papier;

Opis videa syntézy amfetamínu.

Pred začiatkom syntézy sa pripraví roztok 1-fenyl-2-nitropropénu 10 g v 100 ml izopropylalkoholu a 50 ml kyseliny octovej. Taktiež sa skartovačkou papiera nastrúha hliníková fólia 12 g na malé kúsky na prípravu hliníkového amalgámu. Môže sa strihať nožnicami alebo trhať rukami (v rukaviciach).

0:04-0:40 - Vodný roztok alkalického prípravku. Tento roztok bol pripravený vopred, aby mal roztok izbovú teplotu do času alkalizácie hlavnej reakčnej zmesi v tomto videu. Alkalizácia sa vykonáva samovoľným zahrievaním. Ak sa použije čerstvý horúci alkalický roztok, teplota stúpne vyššie a bude potrebné nútené ochladenie reakčnej hmoty.

0:46 - 2:36 - Amalgám s dusičnanom ortuťnatým. Amalgamovaný hliník zredukuje 1-fenyl-2-nitropropén na amfetamín. Počas amalgamačnej reakcie sa uvoľňuje malé množstvo plynu, vzniká sivá zrazenina. Je dôležité nepremeškať okamih, keď je hliníkový amalgám hotový. Tento okamih možno určiť podľa tvorby sivej zrazeniny a zvýšeného vývinu plynu. Stane sa to za 10 až 15 minút od začiatku reakcie.

Voda sa vypustí bez odstránenia gázy, amalgamovaný hliník sa premyje dvoma dávkami studenej destilovanej vody. Je potrebné venovať pozornosť uvoľňovaniu plynových bublín. Všimnite si, že bublinky sú menšie a farba kvapaliny je tmavšia v "správnom" amalgáme. Ak je reakcia prudká, bubliny sú veľké a farba je svetlá, amalgám je "nesprávny". Je to takmer určite spôsobené nedostatkom ortuťovej soli. Upozorňujeme, že ortuťové soli sú jedovaté.

2:37-4:28 - Najdôležitejšoučasťou procesu je redukcia 1-fenyl-2-nitropropénu hliníkovým amalgámom. Reakcia je exotermická a prebieha za výdatného uvoľňovania tepla. Počas postupu je potrebné starostlivo kontrolovať teplotu. Reakčná banka sa v prípade prehriatia chladí v ľadovom kúpeli. Do banky sa môže pridať studená voda. Niekedy sa reakcia nespustí, je potrebné reakčnú hmotu dôkladne zohriať a reakcia sa spustí (so správne pripraveným amalgámom). Počas reakcie sa uvoľňuje zápach vriaceho alkoholu a kyseliny octovej. Na zachytenie pár sa používa Allihn refluxný kondenzátor. Účinnosť Allihn refluxného kondenzátora možno zvýšiť tečúcou studenou vodou, ktorá sa k nemu môže pripojiť.

5:04 - Reakčnú banku možno vypláchnuť malým množstvom alkoholu a nezreagovaný hliník sa ním môže tiež vypláchnuť, aby sa zachytili zvyšky a zvýšil výťažok.

5:13 - Nezreagovaného hliníka by malo zostať málo. Množstvo zreagovaného 1-fenyl-2-nitropropénu môžete určiť podľa zvyškov.

5:16-6:13 - Alkalizácia. Reakcia prebieha s uvoľňovaním tepla. Zvyšky nezreagovaného hliníka dodatočne reagujú so zásadou a zahrievajú zmes, ako aj vytvárajú vedľajšie produkty.
K rozdeleniu na viditeľné vrstvy dochádza do 30 minút po alkalinizácii. pH vrchnej vrstvy by malo byť 11 - 12.

6:18 - 7:23 - Dekantácia. Zoberte vrchnú vrstvu s amfetamínovou bázou v alkohole. Môže sa vysušiť malým množstvom bezvodého síranu horečnatého. Trosku možno extrahovať nepolárnym rozpúšťadlom (éter, benzén, toluén), potom sa rozpúšťadlo odparí.

7:24 - 8:50 - Príprava roztoku kyseliny sírovej v acetóne. Tento roztok je potrebný na hladšie okyslenie. Ak sa použije koncentrovaná kyselina sírová, dôjde k lokálnemu prekysleniu produktu. Preto výťažok klesá.

8:51-10: 53 - Okyslenie produktu a získanie amfetamínsulfátu. K hornej žltej vrstve, ktorá bola zachytená v predchádzajúcej fáze, sa po kvapkách pridá pripravený roztok kyseliny sírovej. S každou kvapkou roztoku kyseliny sa vytvoria vločky soli. Táto fáza je veľmi dôležitá, je potrebné starostlivo kontrolovať pH, aby sa zabránilo nadmernému okysleniu. V okysľovaní sa pokračuje až do pH 5,5 - 6. Prekyslený produkt má ružovkastú farbu. V prípade úplného prekyslenia sa produkt pokazí.

10:55 - 11:38 - Filtrácia amfetamín sulfátu z rozpúšťadiel v Buchnerovom lieviku vo vákuu. Produkt sa môže v tejto fáze dodatočne opláchnuť studeným acetónom tak, že sa preleje cez Buchnerov lievik s koláčom amfetamín sulfátu.

11:41-12:28 - Filtrácia pomocou improvizovaných nástrojov. Ako filter sa môže použiť akákoľvek hrubá tkanina. Výsledný produkt sa niekoľko hodín suší na teplom a suchom mieste, aby sa odstránili zvyšky rozpúšťadiel. Odporúča sa skladovať ho vo vákuovom obale.

Výťažok je 60 - 70 %.

 

[battman23]

Do you have a source to purchase P2NP or point me in the right direction

 

[johan.j]

Is possible use less IPA and less glacial acetic acid in this reaction?

 

[layman]

Existuje nejaký konkrétny dôvod, prečo uprednostniť izopropanol pred etanolom?

 

[lone_w0lf]

I’m not an expert, so take this with a grain of salt, but I assume that isopropyl alcohol in its pure form is more readily available, cheaper, less polar, and less reactive — so it’s probably the more suitable choice.

 

[Letswork2025]

Is 80% acetic acid good enough?

 

[G.Patton]

You can use it but you have to recalculate it and take it more than GAA.

 

[Jordan Belfort]

The stoichiometry is correct ? Isn't it very excess for only 10 grams?

Also what is your opinion about replacing GGA/Acetic acid with Phosphoric acid 85%, replace IPA with methanol (for boiling) and allowing direct extraction with hexane after alkalization -> brine wash till brine no longer takes dirt and simply evaporate the hexane ?

And regarding the foil, I personally suggest 0.03 0.05MM thick (technical aluminium foil) compared to supersmarket householdfoil.
In this reaction, once tried, I must actually check it myself perhaps use even thicker.

 

[G.Patton]

Yes, it is correct.
I'm not sure about phosphoric acid, but for sure you can use formic acid instead. So far as methanol boiling is concerned, it will be the last synthesis you see
Hexane also can be used.

 

[Jordan Belfort]

What do you mean ? 10L MDP2P batches are no problem with thick alu foil and 10 grams mercury chloride per liter MDP2P and little excess methanol. Reaction takes about 4-5 hours and it boils itself slowly, you can even put plastic drum lid on it no stress.

Then hexane extraction and brine wash as usual.

You think there will come explosion with P2NP ? If you think it's really that violent I can use less foil and once the boiling tempreture is reached simply add foil till all is consumed what should be added. But still I find it stunning why we need to use so much glacial acetic acid. Looking at the 'strenght' of for example sulfuric acid, wouldn't that be a better alternative ? As I have read HCL could also be used so why would not be sulfuric acid ?

Do you put a certain stoichemitry, or do you put the post-reaction mixture at a certain pH, before you add the mercury/foil ?

I know a friend of mine used ammonia chloride for MDA synthese I think was also Al/Hg, perhaps is that also a possiblity here ?

Sorry for my little problematic English.

 

[G.Patton]

This discussion not about MDP2P.

You can perform this synthesis even without GAA. Look at this tutorial.
In case of more of 100g P2NP, It will be impossible to control this too violate exothermic reaction and dissipate heat. It can blow up. You can experiment with foil addition but don't think that it will lead to any result due to nature of this reaction.

 

[homestead]

I've tested with 50g p2np and reaction was very controllable, will be scaling up to 100g this week.

 

[Jordan Belfort]

I am going to try larger, did you use cooling or simply 'mexican style' open pot with enough solvent to boil off?

 

[homestead]

Cooling with an icebath

 

[Klefedronek1337]

Can I evaporate water from the electrolyte for the battery and use this sulfuric acid? , Is there a guide maybe on the forum on how to safely evaporate this?

 

[GhostChemist]

http://bbzzzsvqcrqtki6umym6itiixfhn...ntrated-sulfuric-acid-production-at-home.376/

 

[Chemdog010297]

Can I just use sodium chloride instead of sodium thiosulfate for drying solvent ?

 

[GhostChemist]

absolutely no
sodium thiosulphate is Na2S2O3 (may be you mean Na2SO4 sodium sulphate, so it is drying agent)
sodium chloride is not drying agent

 

[tabletopper]

I'm using 99% sulphuric, is this okay to add directly into acetone then added drop wise to a-oil?
Or should I dilute my sulphuric with IPA before adding to acetone??

 

[GhostChemist]

"I'm using 99% sulphuric, is this okay to add directly into acetone then added drop wise to a-oil?" - this way is right. Dissolve 99% sulphuric acid in acetone and add to a-oil (more better dissolve a-oil in aceton too)

 

[tabletopper]

How much acetone if I have 250ml a-oil sir?

 

[tabletopper]

(dissolving a-oil in acetone)

 

[GhostChemist]

1:1 is norm proportions

 

[William Dampier]

You can use a 1ml of sulfuric acid in 5-10ml of dry acetone as an optimally diluted solution for acidification. And add acetone to the oil sparingly, or add it as needed if it thickens.

 

[AntonioManchado]

Hello,

I am starting to make my first syntheses using this system and I have some doubts, I hope you can help me with them:

1. How long do you let the NaOH solution react with the MR? I'm leaving it for about 12 hours so the layers separate properly. Is that okay?

2. Once the top layer has been removed, I measure its pH and I always get a result of 10. Why could it be and I can't get a pH of 11-12?

3. To purify it, I first filter out any solids that may be present through a coffee filter, then I decant it using a funnel and put the resulting liquid in the refrigerator for a few hours to crystallize any impurities that may remain and eliminate them using another filter. Would this be correct? Should I subsequently evaporate the solvent? Did I leave any more steps for purification?

I hope you can help me with this, on the other hand I would like to know if to make, for example, 300 g of P2PNP, it is mandatory to make the amalgam with 30 L of water or this amount of water could be reduced in the reaction. With the IPA and the GAA, should I also use 3 and 1.5 L respectively or could these quantities be reduced?

 

[William Dampier]

You prepare a solution of sodium hydroxide in water in advance, so that the mixture has time to cool down (the reaction is exothermic when mixed with water). Using a cool hydroxide solution would be the most correct. The reaction with the reaction mixture should proceed quite quickly if all the aluminum has reacted or the residue has been filtered off. Then, the separation of the base occurs instantaneously after mixing with the required amount of hydroxide solution (but we add it gradually, of course).

A basic pH of 10 or greater is sufficient for base separation.

You need to distill off the solvent if you have an excess left after the reaction – if it’s an alcohol, it hinders crystallization without adding excess acetone.

The proportions are preferably maintained when scaling up, but the 300g reaction is quite specific and requires a disproportionate increase in reaction volume and certain experience to control the reaction. Furthermore, the yield is usually lower than when making smaller batches. This can be corrected, but it requires equipment.

 

[AntonioManchado]

So, is it better to use a cold NaOH solution from the refrigerator rather than at room temperature? Should we also let the RM cool down?

You mentioned that it's best to distill the solvent. I'm evaporating mine at 40-50°C, but I'm worried that if I increase the temperature, the oil will decompose. Is that correct too?

Regarding pH: if it's 10, why is it said that oil with a pH of 11.7 is better? Is that true? How could I achieve that pH of 11.7, for example, by adding 60g of NaOH to 10g of P2NP instead of the current 50g?

Is it normal for the oil to crystallize, or are those impurities?

How can I tell if my oil is of good quality? By its density? Boiling point?

With your help, I'm on the right track. Thank you.

 

[William Dampier]

At least to room temperature. It can be cooled further, but so as not to get sodium hydroxide crystallization back.

Distillation of the solvent is not always necessary. You can apply this if you have problems with crystallization. Or if you want to obtain pure a-oil for transportation. However, for such distillation, it is desirable to dry the solution to avoid losing the base due to the distillation of water particles. Then, use vacuum distillation for better and faster separation. If necessary for purity, the base itself can be distilled.

Approximately 50g of NaOH is usually sufficient for 10g of P2NP. Otherwise, the quantity will vary depending on the reaction mixture, residual aluminum, and so on.

For pure base without solvents, crystallization is possible when lowering the temperature (below the melting point).