Amphetamine synthesis from P2NP via Al/Hg (video)

[HIGGS BOSSON]

In the video synthesis of amphetamine, reagents are used:

• 10 g 1-Phenyl-2-nitropropene (P2NP);
• 100 ml Isopropyl alcohol (IPA);
• 50 ml Glacial acetic acid (AcOH);
• 50 g Sodium hydroxide (NaOH);
• 12 g Aluminium (in the form of sliced household foil);
• 0.1g Mercury (II) nitrate (Hg(NO3)2);
• 2 ml Sulphuric acid (H2SO4);
• 50 ml Acetone;
• Distilled water;

Equipment and glassware:

• Flat bottom flask 2 L;
• Retort stand and clamp for securing apparatus (optional);
• Reflux condenser;
• Funnel;
• Sieve filter (kitchen grade is ok);
• Syringe or Pasteur pipette;
• pH indicator papers;
• Beakers (600 mL x2, 2 L, 1 L, 100 mL x2);
• Vacuum source;
• Laboratory scale (0.1-200 g is suitable);
• Measuring cylinders 1000 mL and 100 mL;
• Cold water bath;
• Glass rod and spatula;
• Separatory funnel 1 L (optional);
• Laboratory grade thermometer;
• Buchner flask and funnel;
• Filter paper;

​

Description of amphetamine synthesis video.

A solution of 1-phenyl-2-nitropropene 10 g in 100 ml of isopropyl alcohol and 50 ml of acetic acid is prepared before the synthesis start. Also, an aluminium foil 12 g is cut into small pieces with a paper shredder for an aluminium amalgam preparation. It can be cut with scissors or torn by hands (in gloves).

0:04-0:40 - An aqueous alkali solution of preparation. This solution was made in advance so that the solution has room temperature by the main reaction mixture alkalization time in this video. The alkalinization is carried out with a spontaneous heating. If a fresh hot aq alkali solution is used, then the temperature is risen higher and a reaction mass forced cooling will be required.

0:46-2:36 - Amalgam with mercury nitrate. Amalgamated aluminium will reduce 1-phenyl-2-nitropropene to amphetamine. A small amount of gas is evolved during the amalgamation reaction, a grey precipitate is formed. It is important not to miss the moment when the aluminium amalgam is ready. This moment can be determined by a grey precipitate formation and by an increased gas evolution. It happens in 10-15 minutes from reaction start.

The water is drained without a gauze removing, the amalgamated aluminium is washed with two portions of cold distilled water. It is worth to pay attention to a gas bubbles releasing. It is noticed that bubbles are smaller and liquid color is darker in a "correct" amalgam. If the reaction is violent, bubbles are large and the color is light, the amalgam is "incorrect". This is almost certainly due to a lack of mercury salt. Please note that mercury salts are poisonous.

2:37-4:28 - The most important part of the process is 1-phenyl-2-nitropropene reduction by aluminium amalgam. The reaction is exothermic and carried out with an abundant heat releasing. It is necessary to carefully control the temperature during the procedure. Reaction flask is cooled in an ice bath in case of overheating. It is allowed to add cold water into the flask. Sometimes the reaction isn't started, it is necessary to warm the reaction mass thoroughly and the reaction is started (with a properly prepared amalgam). Smells of a boiling alcohol and acetic acid are released during reaction. Allihn reflux condenser is used for a vapors capturing. The efficiency of Allihn reflux condenser can be increased by a running cold water, which can be connected to it.

5:04 - The reaction flask can be rinsed with a small amount of alcohol and unredacted aluminium can be rinsed with it as well for collecting residues and increasing the yield.

5:13 - There should be little unreacted aluminium left. You can determine an amount of reacted 1-phenyl-2-nitropropene by the residues.

5:16-6:13 - Alkalinization. The reaction is conducted with a heat releasing. The remains of unredacted aluminium will additionally react with alkali and heat the mixture as well as create by-products.
A separation into visible layers occurs within 30 minutes after alkalinization. The pH of the top layer should be 11-12.

6:18-7:23 - Decantation. Collect the top layer with amphetamine base in alcohol. It can be dried by a small amount of anhydrous magnesium sulfate. The slag can be extracted with a non-polar solvent (ether, benzene, toluene), then a solvent is evaporated.

7:24-8:50 - Preparation of the sulphuric acid solution in acetone. This solution is necessary for smoother acidification. If concentrated sulphuric acid is used, local over-acidification of the product is happened. Hence, the yield is dropping.

8:51-10:53 - Product acidification and amphetamine sulfate obtaining. To the upper yellow layer, which was collected at the previous stage, a prepared solution of sulphuric acid is added dropwise. Flakes of salt are formed with each drop of acid solution. This stage is very important, it is necessary to carefully control pH to avoid over-acidification. Acidification is continued until pH 5.5-6. The over-acidified product has pinkish color. The product will be spoiled in case of a total over-acidification.

10:55-11:38 - Amphetamine sulfate filtration from solvents in a Buchner funnel under vacuum. The product can be additionally rinsed with cold acetone at this stage by pouring it through Buchner funnel with the amphetamine sulphate cake.

11:41-12:28 - Filtration using improvised tools. Any thick fabric can be used as a filter. The resulting product is dried in a warm dry place for several hours to remove residual solvents. It is recommended to store it in a vacuum package.

The yield is 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]

Is there any specific reason to prefer isopropanol over ethanol?

 

[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).