Amphetamine synthesis from P2NP via Al/Hg (video)

[Gale]

It is always better to use as anhydrous solvent as possible if the obtained salt dissolves well in water, it increases the yield.

PennywiseOk to dry the ipa/H₂SO₄ with MgSO₄? I think the what I can get is 92-96% h2s04

 

[cyb3r0]

. When reducing the amount of p2np to 5g. What are the correct proportions of other reagents.

 

[Mclssmxxl]

. When reducing the amount of p2np to 5g. What are the correct proportions of other reagents.

cyb3r0They scale linearly, so half of everything.Reflux is not obligatory to happen for reaction to take place, if you control the reaction properly in an appropriate flask with a beefy condenser it won’t reach reflux even, especially aith 5g.If you reaction is not starting at all however with the addition of your propene, I would maybe check : if amalagam was done correctly, the purity of my raw materials (especially the propene).And ffs use distilled.

 

[ACAB]

Ok to dry the ipa/H₂SO₄ with MgSO₄? I think the what I can get is 92-96% h2s04

GaleNormally, one does not dry concentrated sulfuric acid at all, but uses it to dry itself.

If I mix 1ml H2SO4 96% and 5ml dry IPA for titration, I have approx. 0.04ml water in the solution. In such a constillation I think there is no reason to use desiccant.
It will certainly not do any harm, but it is questionable whether it will work.

 

[Gale]

When the mixture reacts, there is no reflux process, why?

cyb3r0
If it doesn't start bulbbing and heating up with foil then sum-ting-wong

 

[Gale]

I've been having issues with PMK all/hg reduction, I have a large amount of unreacted aluminium leftover after a 240g ketone rxn. The vessel heated on its own with reflux to around 65c and dropped to 40c over the course of 90mins. Then heat was applied to bring it up to 50-60c for 3-4 hours.

Pie pans were used and cut into 1 cm small strips and 10% excess was added to osmium writeup. After basifying the ai was reduced. Then goods extracted with toluene and washed with naoh solution. I'm hoping for atleast 100g yeild. If not then I'm fucked and will have to save some more money for another rxn and just used foil so it gets eaten.

I recall there being maybe 50% ai leftover. This was 100% aluminium disposable baking pans. I waited about 45-60mins for amalgamation to start and only a few pieces were floating, I assumed its because its thicker ai..but there was bubbling going on the the solution had a silvery appearance.. It seemed ready. And the rxn heated to 65c on its own so I'm sure it was ready...maybe I just have to gas and see the yeild...I have a feeling it going to be bad lol. D
oes osmium already add extra aluminium? Maybe I added excess on excess lol. Anyways I think thick foil would be OK for 200-300g reduction. I wish I realized this and stuck with foil on these larger rxns...but this is how I learn. If the reaction went to 65c with Al pans then with foil it might be too exothermic right? So my Al thickness might be on point and maybe I have to let amalgamate longer until all pieces are floating? it seemed to me like it was going and exothermic reaction kicked in.

If been wasting quite a bit of material and time on trying to scale up and each time I'm playing around with thicker Al, when I think I should stick to maybe a thicker foil, that way it all gets consumed and the temps may go up to like 75c but can cool it to keep under 70 no problem. If I knew about the NMF route before preparing for osmium route then I would being using NMF and I think I'd have less problems.
I will report back with yeild on the pie pan run.

 

[cyb3r0]

The product came out with me like this as hair!

 

[cyb3r0]

If it doesn't start bulbbing and heating up with foil then sum-ting-wong

GaleSorry what do you mean by sum-ting-wong

 

[cyb3r0]

What is the thickness of aluminum foil suitable?

 

[Gale]

What is the thickness of aluminum foil suitable?

cyb3r0IMO any Al thick foil is good depending on your scale. Store bought heavy duty foil for doing small scale and even bigger reactions but the All granules or Al fine CNC shavings looks nice.

I'm.not familiar with amphetamine but that could be your drying agent possibly. If its your yeild than it looks OK to me.

 

[cyb3r0]

Did I use any capacitors in this synthesis, or are there specific capacitors? Thank you

 

[AstekPL]

the synthesis was carried out as in the movie, the product has no power. What to do?

 

[WillD]

the synthesis was carried out as in the movie, the product has no power. What to do?

AstekPLDoes the product have a salty taste or is it bitter?

 

[cyb3r0]

When you taste the product at first, it will taste very salty, and in the end, amphetamine taste appears

 

[Catweazle]

In the video synthesis of amphetamine, reagents are used:
10 g 1-phenyl-2-nitropropene;
100 ml isopropyl alcohol;
50 ml glacial acetic acid;
50 g sodium hydroxide;
12 g aluminium (in the form of sliced household foil);
0.1g mercury nitrate;
2 ml sulphuric acid;
50 ml acetone.

Description of amphetamine synthesis video.
Before the start of the synthesis, the laboratory assistant prepared a solution of 10 g of 1-phenyl-2-nitropropene in 100 ml of isopropyl alcohol and 50 ml of acetic acid. Also, for the aluminium amalgam, 12 g of household aluminium foil was prepared, which was cut into small pieces with a paper shredder. It can be cut with scissors or torn by hand.

0:04-0:40 - Preparation of an aqueous solution of alkali. In this video, it was made in advance so that the solution cools down by the time the main reaction mixture alkalizes. Alkalinization proceeds with the release of heat, and if a fresh hot alkali solution is used, then the exothermic will be more pronounced and forced cooling of the reaction mass will be required.

0:46-2:36 - Amalgam of mercury nitrate. Amalgamated aluminium will reduce 1-phenyl-2-nitropropene to amphetamine. During the amalgamation reaction: little gas evolves, a grey precipitate is formed. It is important not to miss the moment when the aluminium is ready: this can be determined by the formation of a grey precipitate and by the increased gas evolution; this happens in 10-15 minutes after the load.
The water is drained without removing the gauze, the amalgamated aluminium is washed with two portions of cold water. It is worth paying attention to the release of gas bubbles: it is noticed that with the "correct" amalgam, these bubbles are small, and the colour of the liquid is darker; if the bubbles are large and the colour is light, and the reaction looks violent, the amalgam is bad. 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 the reduction of 1-phenyl-2-nitropropene on aluminium amalgam. The reaction is exothermic, proceeds with abundant heat release. During the process, it is necessary to carefully monitor the temperature, in case of excessive overheating, to cool in an ice bath, it is allowed to add cold water to the flask. There are cases when the reaction does not start, in which case it is necessary to warm the reaction mass thoroughly, and with a properly prepared amalgam, the reaction begins. The reaction proceeds with the release of the smell of a boiling alcohol and acetic acid mixture. To capture vapours, a spherical irrigation condenser is used, the efficiency of which can be increased by connecting running cold water to it or simply pouring cold water into.

5:04 - You can rinse the flask with a little alcohol and rinse the unreacted aluminium with it to collect residues and increase the yield.

5:13 - There should be little unreacted aluminium left. By the residues, you can determine the amount of 1-phenyl-2-nitropropene reacted.

5:16-6:13 - Alkalinization. The reaction proceeds with the release of heat. The remains of unreacted aluminium will additionally enter into reaction with alkali and heat the mixture, as well as create by-products.
In the process of allowing the mixture to rest after alkalinization, separation into visible layers occurs within 30 minutes. The pH of the top layer should be 11-12.

6:18-7:23 - Decantation: collect the top layer containing amphetamine base in alcohol. It can be dried a little with anhydrous magnesium sulfate, and the slag can be additionally extracted with a non-polar solvent (ether, benzene, toluene), the solvent is then evaporated.

7:24-8:50 - Preparing a solution of sulphuric acid in acetone. It is made softer acidification of the product to be smoother. If concentrated sulphuric acid is used, there may be local over-acidification of the product.

8:51-10:53 - Product acidification - obtaining amphetamine sulfate. To the upper yellow layer collected at the previous stage, a prepared solution of sulphuric acid is added dropwise. Flakes of salt will form with each drop. This stage is very important, it is necessary to carefully monitor the pH, avoiding over-acidification. Acidification is continued until pH 5.5-6 (neutral). The over-acidified product will be pinkish in colour. In case of global over-acidification, the product will be lost.

10:55-11:38 - Filtration of amphetamine sulfate from solvents in a Buchner funnel under vacuum. At this stage, the product can be additionally rinsed with cold acetone by pouring it through the funnel with the substance.

11:41-12:28 Filtration using improvised means. 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%.

HIGGS BOSSONHi
Would dcm or chloroform be a suitable solvent.

 

[ASheSChem]

5:04 - You can rinse the flask with a little alcohol and rinse the unreacted aluminium with it to collect residues and increase the yield.

HIGGS BOSSONIsopropanol is ok i presume ?
we rinse the ballon, and put the the result on the fine sieve for going with the rest before alkalinization ?
no need to evaporate isopropanol or something like that ? (any idea of max isopropanol quantity we can use for the rinse?)

 

[diogenes]

When you taste the product at first, it will taste very salty, and in the end, amphetamine taste appears

cyb3r0It can be Sodium Sulphate... Your reaction might not have gone all the way through. I had the same issue in the beginning, had Na2SO4 as well and others. The solution was not to rinse the amalgam (just draining the water) and also my rule for the readiness is when all the Al comes up to the surface and you can also hear a sizzling sound. There are also small bubbles appearing. This is when I consider ithe amalgam ready, and this solved the lack of reaction problem. My yield varies usually only around 50%, but never had a non-reactive amalgam since then.

 

[cyb3r0]

It can be Sodium Sulphate... Your reaction might not have gone all the way through. I had the same issue in the beginning, had Na2SO4 as well and others. The solution was not to rinse the amalgam (just draining the water) and also my rule for the readiness is when all the Al comes up to the surface and you can also hear a sizzling sound. There are also small bubbles appearing. This is when I consider ithe amalgam ready, and this solved the lack of reaction problem. My yield varies usually only around 50%, but never had a non-reactive amalgam since then.

diogenesExcuse me . But we did not use sodium sulfate in this synthesis. What is its relationship to the topic? If you would allow, please explain to me more. I did not understand the idea. Thank you

 

[diogenes]

Excuse me . But we did not use sodium sulfate in this synthesis. What is its relationship to the topic? If you would allow, please explain to me more. I did not understand the idea. Thank you

cyb3r0Hi, I`m not an expert by any means, so others might confirm or correct this, but when you add sulphuric acid (H2SO4) to the mixture if there is no amphetamine base present (i.e. the reduction did not happen) then the SO4 might form a salt with the Sodium (Na). The Sodium is present in the solution from the NaOH added earlier.

 

[diogenes]

To the experts: What happens if we use more Al foil in the reaction? Could it increase the yield?