Amfetamīna sintēze no P2NP, izmantojot Al/Hg (video)

[HIGGS BOSSON]

Video amfetamīnasintēzē tiek izmantoti reaģenti:

• 10 g 1-fenil-2-nitropropēna (P2NP);
• 100 ml izopropilspirta (IPA);
• 50 ml ledus etiķskābes (AcOH);
• 50 g nātrija hidroksīda (NaOH);
• 12 g alumīnija (sagrieztas sadzīves folijas veidā);
• 0,1 g dzīvsudraba (II) nitrāta (Hg(NO3)2);
• 2 ml sērskābes (H2SO4);
• 50 ml acetona;
• Destilēts ūdens;

Iekārtas un stikla trauki:

• Kolba ar plakanu dibenu, 2 l;
• Retorta statīvs un skava aparāta nostiprināšanai (pēc izvēles);
• Atpakaļplūsmas kondensators;
• piltuve;
• sieta filtrs (der virtuves filtrs);
• Šļirce vai Pastēra pipete;
• pH indikatora papīriņi;
• spaiņi (600 ml x2, 2 L, 1 L, 100 ml x2);
• Vakuuma avots;
• Laboratorijas svari (piemēroti 0,1-200 g);
• Mērcilindri 1000 ml un 100 ml;
• Aukstā ūdens vanna;
• Stikla stienis un lāpstiņa;
• 1 L dalāmā piltuve (pēc izvēles);
• laboratorijas termometrs;
• Bihnera kolba un piltuve;
• filtrpapīrs;

Amfetamīna sintēzes video apraksts.

Pirms sintēzes sākuma sagatavo 10 g 1-fenil-2-nitropropēna šķīdumu 100 ml izopropilspirta un 50 ml etiķskābes. Alumīnija amalgamas pagatavošanai arpapīra smalcinātāju sagriež sīkos gabaliņos arī alumīnija foliju 12 g . To var sagriezt ar šķērēm vai pārgriezt ar rokām (cimdos).

0:04-0:40 - Preparāta ūdens sārma šķīdums. Šis šķīdums tika pagatavots iepriekš, lai šķīdumam būtu istabas temperatūra līdz galvenajam reakcijas maisījuma sārmošanas laikam šajā video. Sārmošanu veic ar spontānu sildīšanu. Ja izmanto svaigu karstu sārmu šķīdumu, tad temperatūra paaugstināsies un būs nepieciešama reakcijas masas piespiedu dzesēšana.

0:46-2:36 - Amalgama ar dzīvsudraba nitrātu. Amalgamētais alumīnijs reducē 1-fenil-2-nitropropēnu līdz amfetamīnam. Amalgamēšanas reakcijas laikā izdalās neliels gāzes daudzums, veidojas pelēkas nogulsnes. Ir svarīgi nepalaist garām brīdi, kad alumīnija amalgama ir gatava. Šo brīdi var noteikt pēc pelēko nogulšņu veidošanās un pastiprinātas gāzes izdalīšanās. Tas notiek 10 līdz 15 minūšu laikā no reakcijas sākuma.

Ūdens tiek izlaists bez marles noņemšanas, amalgamētais alumīnijs tiek izskalots ar divām porcijām auksta destilēta ūdens. Jāpievērš uzmanība gāzes burbuļu izdalīšanai. Novēro, ka "pareizā" amalgamā burbuļi ir mazāki un šķidruma krāsa ir tumšāka. Ja reakcija ir strauja, burbuļi ir lieli un krāsa ir gaiša, amalgama ir "nepareiza". Tas gandrīz noteikti ir saistīts ar dzīvsudraba sāls trūkumu. Ņemiet vērā, ka dzīvsudraba sāļi ir indīgi.

2:37-4:28 - Vissvarīgākā procesa daļa ir 1-fenil-2-nitropropēna reducēšana ar alumīnija amalgamu. Reakcija ir eksotermiska, un tā notiek, izdalot daudz siltuma. Procedūras laikā rūpīgi jākontrolē temperatūra. Reakcijas kolbu pārkaršanas gadījumā atdzesē ledus vannā. Kolbā drīkst pievienot aukstu ūdeni. Dažreiz reakcija netiek uzsākta, reakcijas masa kārtīgi jāsasilda un reakcija jāuzsāk (ar pareizi sagatavotu amalgamu). Reakcijas laikā izdalās verdoša spirta un etiķskābes smarža. Tvaiku uztveršanai izmanto Allihn atgaitas kondensatoru. Allihn pretplūsmas kondensatora efektivitāti var palielināt, ja tam pieslēdz tekošu aukstu ūdeni.

5:04 - Reakcijas kolbu var izskalot ar nelielu daudzumu spirta, un ar to var izskalot arī nereaģējušo alumīniju, lai savāktu atlikumus un palielinātu iznākumu.

5:13 - Nereaģējušajam alumīnijam jābūt maz. Pēc atlikumiem var noteikt reaģējušā 1-fenil-2-nitropropēna daudzumu.

5:16-6:13 - Sārmojums. Reakciju veic ar siltuma izdalīšanu. Nereaģējušā alumīnija atliekas papildus reaģē ar sārmu un maisījumu uzkarsē, kā arī rada blakusproduktus.
30 minūšu laikā pēc sārmošanas notiek atdalīšanās redzamos slāņos. Augšējā slāņa pH jābūt 11-12.

6:18-7:23 - Dekantēšana. Savāc virsējo slāni ar amfetamīna bāzi spirtā. To var izžāvēt ar nelielu daudzumu bezūdens magnija sulfāta. Šlakvielas var ekstrahēt ar nepolāru šķīdinātāju (ēteri, benzolu, toluolu), tad šķīdinātāju iztvaicē.

7:24-8:50 - Sērskābes šķīduma sagatavošana acetonā. Šis šķīdums ir nepieciešams vienmērīgākai paskābināšanai. Ja izmanto koncentrētu sērskābi, notiek vietēja produkta pārskābošanās. Tādējādi samazinās iznākums.

8:51-10: 53 - Produkta paskābināšana un amfetamīna sulfāta iegūšana. Augšējam dzeltenajam slānim, kas tika savākts iepriekšējā posmā, pilienveidā pievieno sagatavotu sērskābes šķīdumu. Ar katru pilienu skābes šķīduma veidojas sāls pārslas. Šis posms ir ļoti svarīgs, rūpīgi jākontrolē pH, lai izvairītos no pārskābes. Skābināšanu turpina līdz pH 5,5 - 6. Pārskābinātam produktam ir sārta krāsa. Pilnīgas pārskābes gadījumā produkts bojājas.

10:55-11:38 - Amfetamīna sulfāta filtrēšana no šķīdinātājiem Bihnera piltuvē vakuumā. Šajā posmā produktu var papildus noskalot ar aukstu acetonu, izlejot to caur Buknera piltuvi kopā ar amfetamīna sulfāta kūku.

11:41-12:28 - Filtrēšana, izmantojot improvizētus instrumentus. Par filtru var izmantot jebkuru biezu audumu. Iegūto produktu vairākas stundas žāvē siltā un sausā vietā, lai atdalītu šķīdinātāju atliekas. Ieteicams to uzglabāt vakuuma iepakojumā.

Ieguvums ir 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]

Vai ir kāds īpašs iemesls, kādēļ izopropanolam dot priekšroku etanolam?

 

[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).