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Synthesis of amphetamine from P2NP via Al/Hg (video)

ACAB

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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.
Yes, that will always works right, but you will never get the same yield on a regular basis because it is a gamble unless you have a decent amalgam. After all, I have the same problem. An optimal reaction would be to convert the aluminum completely into amalgam, i.e. add exactly the right amount of mercury salt and then after the reduction, have no solid aluminum/amalgam left in the flask, because thus everything has been converted with P2NP.
It simply makes more sense to wait the first time after adding mercury salt until it has reacted completely, i.e. no more bubbles are formed, and then to start the reduction of P2NP with new mercury salt and residual aluminum that is certainly still in the flask. If the reduction stops and there is still aluminum in the flask, a further addition of mercury salt would be necessary to convert these residues with P2NP.
I think this is the way we should go, after all I have learned here.
 

diogenes

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Yes, that will always works right, but you will never get the same yield on a regular basis because it is a gamble unless you have a decent amalgam. After all, I have the same problem. An optimal reaction would be to convert the aluminum completely into amalgam, i.e. add exactly the right amount of mercury salt and then after the reduction, have no solid aluminum/amalgam left in the flask, because thus everything has been converted with P2NP.
It simply makes more sense to wait the first time after adding mercury salt until it has reacted completely, i.e. no more bubbles are formed, and then to start the reduction of P2NP with new mercury salt and residual aluminum that is certainly still in the flask. If the reduction stops and there is still aluminum in the flask, a further addition of mercury salt would be necessary to convert these residues with P2NP.
I think this is the way we should go, after all I have learned here.
Correct me if I`m wrong, but we cannot wait until the reaction is complete, because then all the Aluminium will be used up and convertec in to Al:

{\displaystyle {\ce {2Al + 3Hg^2+ + 6H2O -> 2Al(OH)3 + 6H+ +3Hg}}}

{\displaystyle {\ce {Hg + Al -> Hg*Al}}}

{\displaystyle {\ce {2 Hg*Al + 6 H2O -> 2 Al(OH)3 + 2 Hg + 3 H2}}}

There must be an `ideal moment` when most of the Al is in HgAl form which is the form capable of reducing P2NP to amphetamine base. It is the generation of H2 which causes the bubbles and it will be present until all the Al is converted into 2Al(OH)3 rendering the Al unreactive.

Perhaps the initial amount of HgNO3 (or HgCl2) needs to be carefully chosen so that the Hg will be enough to have the maximum amount of HgAl at one point. If there is no foil left at all at the end of the reduction of the P2NP then there is a risk of leaving unreacted P2NP.
 

ACAB

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There must be an `ideal moment` when most of the Al is in HgAl form which is the form capable of reducing P2NP to amphetamine base. It is the generation of H2 which causes the bubbles and it will be present until all the Al is converted into 2Al(OH)3 rendering the Al unreactive.
I think that no more bubbles will form as soon as the part of the aluminum has reacted that was accessible, there are no molecules floating in the water, aluminum is a metal that must be removed in layers, figuratively speaking. This means that there is still enough convertible aluminum under the layer to react to HgAl and then to reduce the P2NP, i.e. the chain reaction comes to an end as soon as the surface of the foil has been scratched. Then the water is drained off and the amalgam forms an oxide layer in conjunction with the atmospheric oxygen, which makes the amalgam non-reactive again. Our P2NP solution is added and we do not have a reactive amalgam available, so we again add a lot of mercury salt which starts the reaction and reduction, visible by the many small bubbles that appear until the P2NP is reacted.
We usually have an excess of foil in there to convert all the P2NP, but if there is a lot more aluminum left at the end, the reduction is not complete and not all the P2NP has been converted which means less yield and that means we have not formed enough amalgam to convert it all. What we do if we don't wait until no more bubbles rise during amalgamation.
My opinion, I don't know it.
Perhaps the initial amount of HgNO3 (or HgCl2) needs to be carefully chosen so that the Hg will be enough to have the maximum amount of HgAl at one point. If there is no foil left at all at the end of the reduction of the P2NP then there is a risk of leaving unreacted P2NP.
No aluminum and no feasible P2NP would be the theoretical optimum, which will never be achieved.
 

BlueSolomon

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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%.
Hey, buddy thank you very much for this vid, really amazing, I am not a chemist so I have a ton the doubts the most important being: I don't want to fuck with aluminum on the final product and less with any mercury salts, so my question: if the point of this is making the reduction using free hydrogen, why not use a hydrogen cylinder and sparge hydrogen on the isopropanol + p2np solution. I know this question must be super silly, but as I told you I am not a chemist and I would like to avoid doing the amalgam thing, infinite thanks to all you on this forum and specially the guy whom upload the vid + instructions.
 

DocX

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Hydrogen gas is BAAD, mmkey? Goes boom very easily. And the point is not the hydrogen gas, it's the reduction that is the point. The hydrogen gas is produced as a side product of that reaction.
There is another route using Sodium Borohydride and Copper Chloride. Suitable for smaller batches.
HERE IT IS
No mercury, no aluminum.

But this is the easiest way. What's your problem with aluminum? It's not toxic.
Mercury nitrate is nasty, sure, but if you rinse and recrystallize your final product well, you shouldn't have any residue enough to poison anyone even by i.v use.
 

diogenes

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Mercury nitrate is soluble in Acetone, so an acetone wash at the end should eliminate the rest. It is also insoluble in alcohols so there should not be much in the final product anyway.
 

aladdin_2

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i also want some information on what step(s) of this procedure prevent mercury contamination in the final product, and what further steps can be done to prevent possible contamination? all writeups of similar al/hg reductions always stress the danger of handling water soluble mercury salts but almost NEVER discuss possible contamination... why?

Mercury nitrate is soluble in Acetone, so an acetone wash at the end should eliminate the rest. It is also insoluble in alcohols so there should not be much in the final product anyway.
sure, but am i incorrect and thinking that mercury nitrate is not regenerated at the end of the reduction? it should be mercury metal that remains after all of the aluminum has been consumed and converted to Al(OH)3. assuming the prepared amalgam in the beginning was washed well to remove the mercury salt, the possible sources of mercury contamination would be (1) mercury metal present at reaction end and (2) unreacted amalgamated mercury.

given the ubiquity of this procedure and a lack of mercury poisoning cases in the news related to use of substances prepared in this method, it seems the procedure is fairly airtight with respect to mercury contamination in final product, but can someone explain why? i can understand any elemental mercury being fairly easy to remove given its density as a liquid, but what about the possibility of unreacted amalgamated mercury?
 

diogenes

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all writeups of similar al/hg reductions always stress the danger of handling water soluble mercury salts but almost NEVER discuss possible contamination... why?
Because the risk of poisoning is way higher during the synthesis when handling toxic mercury salts than when consuming the final product. Aluminium amalgam is very reactive and is already changed into mercury at the end of the synthesis. Elemental mercury is not too toxic when ingested orally, it is much worse to inhale its fumes.

Whenever I tried to wash the amalgam (even once let alone X3) the reaction stopped, perhaps I am still not choosing the right moment and there could be a point when the amalgam would even survive washing (it would be extremely helpful and much appreciated if someone more experienced posted pictures or a short video showing sings of this ideal moment).

On the other hand I see very little chance of the Mercury salt getting into the final product. It is not soluble in IPA and then there is Acetone. I usually wash two times during the filtering process. There is very little chance of contamination.

Two related questions to the experts/anyone who knows the answer:

1. Is there an accesible analytical method to quantifty contamination from either the sample or from plasma?
2. Does anyone know a way to `disarm` the filtered fluid? I don`t feel comfortable contacting any organisation, because this way we would end up on some list and under surveillance. Does anyone do some Mercury elimination at home?
 

diogenes

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Mr Patton, if you hear this, please tell us whether a Raman could identify Mercury nitrate from the end product?
 

cyb3r0

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I have expired mercury nitrate, does this affect the quality of the synthesis?
 

G.Patton

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Mr Patton, if you hear this, please tell us whether a Raman could identify Mercury nitrate from the end product?
Hi, depends on power of the laser. In my opinion, better to solve your product in water and pay for water analysis for Hg metal. It's the simplest and the chicest way. Nobody would check your water for organic substances if you pay for metal only.

P.S. Answer me in comments or call me via @, i'll see it faster.
 

cyb3r0

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The amalgam reaction with nitropropene works for the first 5 minutes, and then there is no reaction, so what is the reason?
 

Saul

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hello I use sulphuric acid 96% pure
is this the same as this guy use ?
 

Mclssmxxl

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hello I use sulphuric acid 96% pure
is this the same as this guy use ?
I don’t know what he uses but 96% is fine, just be careful when adding it to solvent, it splashes on contact.
 

ACAB

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I have expired mercury nitrate, does this affect the quality of the synthesis?
Ever heard that salt lies 7 million years in the earth, then it is mined and it is only 2 years shelf life?
The amalgam reaction with nitropropene works for the first 5 minutes, and then there is no reaction, so what is the reason?
Normally this is a chain reaction that only stops when one of the substances is no longer available, I would say that amalgam is missing because it is too poorly prepared, or because an oxide layer is covering the amalgam again, that could be a possibility for example. Have you ever tried to start the reduction again with some mercury salt?
 

William Dampier

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The amalgam reaction with nitropropene works for the first 5 minutes, and then there is no reaction, so what is the reason?
Add more mercury and time until propene is added. Make sure there is enough water or acid in the mixture to produce hydrogen
 

Saul

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I don’t know what he uses but 96% is fine, just be careful when adding it to solvent, it splashes on contact.

I use it also with A-oil but never pure I did for 100ml oil 10 gr 96% and 17gr water it is still much better than the 37% you find everyware
reaction is much better if you mix it just before you use it .
 

Mclssmxxl

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I use it also with A-oil but never pure I did for 100ml oil 10 gr 96% and 17gr water it is still much better than the 37% you find everyware
reaction is much better if you mix it just before you use it .
Are you precipitating with water? The sulphate form is water soluble.From what I understand an anhydrous or nearly anhydrous solvent should be used.
How are your yields?
 
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