Amphetamine synthesis from P2NP via Al/Hg (video)

HIGGS BOSSON

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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;

7sbroyikpe

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%.
 
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timeandtime

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8:51 - what's the shelf life of the clear oil after it's been separated?
 

G.Patton

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I can help you with synthesis, you can ask me in private messages any question about.
 

Barterpayne

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Hi Mister G Patton , after the Aluminum Amalgated with mercury ,
It is said we have to make : P2np + IPa + glacial acetic acid .


Can we replace the acetic acid with Citric Acid ?
In which quantity?
 

William D.

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The usual replacement is formic acid, if it’s so easier. You can buy food vinegar the same way.
 

Eddybeaumont

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hello and thank you for this fabulous video. Is it possible to replace mercury (II) nitrate with mercury (II) chloride for amalgamation with aluminum? If so, does the quantity change? if yes in what quantity for the same proportion as in the video please? thank you in advance for your response
 

G.Patton

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Yes, it's said above and every post about amalgam production. Same molar ration, you need to recount quantity in grams.
 

golab071

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Would it make sense, when producing larger quantities of the product, to use solvents like DMSO (boiling point: 189°C) or toluene (110°C) instead of IPA (82°C), and to place pieces of broken porcelain in the reactor to stabilize the reaction?
 

G.Patton

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The reaction is too violate and exothermic. It think, it have no sense.
 

William D.

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DMSO at high temperature and the presence of acid will begin to degrade on DMS and release oxygen as an oxidizing agent. We have a strong release of hydrogen, which in the aggregate can give "explosive gas". Gently with experiments! In addition, DMSO itself is very smelly with high-temperature synthesis in the presence of many components. Try ethylacetate.
 

Barterpayne

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Please , ithe video shows 12grams of aluminum into a 2000ml flask .
But I wanted to go 24 grams of aluminum grit into the 2000 ml Flask
Please tell me what is ratio for all quantity of other components.

Is it 2 times more IPA ? Glacial acetic acid ? Sulfuric acid ? H2o ? Caustic soda ? And also what about the
Time for reaction ? Does time of reaction also double ? What about decantation when we double quantity for same glassware ?
( Attached the picture of 24 grams of aluminum into a 2 liter flask .)
Please respond need tour help to start
 

G.Patton

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Hi, you need bigger flask. Multiply everything twice. Time is about the same.

Start with smaller amount at first.
 
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Barterpayne

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Mister Patton , can I replace IPA by ethanol , to dissolve P2np for the main reaction into the synthesis '

How much is equivalent of Ethanol to replace 100 ml of IPA for this synthesis
 

G.Patton

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Yes, you can. Same, I guess. You have to dissolve al P2NP.
 

William D.

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You can use various solvents, we even synthesized in ethyl acetate (without acetic acid and alcohol). I think this drawback is solved in the process of hydrolysis when heated in the reaction mixture.
 

William D.

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In 10L flask it is better not to synthesize more than 80g p2np. For 2L flask are similar - it is better not to synthesize more than 15g and in the presence of experience. With experience, you can better control the reaction, but the amount of the above will be a great risk.
 

nofuckups

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What's the exact process of making the P2NP+IPA+GAA solution? Is it just mixing the appropriate quantity of each compound in a beaker, stirring it a bit and then letting it cool? I'm not sure why this part was skipped from the video.
 

G.Patton

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yes, exactly.
 

William D.

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When it has cooled by part of the P2NP can crystallize again. You can add this precipitate to the flask without dissolution or wash off an additional amount of IPA.
 

nofuckups

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or just warming up the entire solution a bit before pouring into the aluminium amalgam?
 

timeandtime

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8:51 - what's the shelf life of the clear oil after it's been separated?
 

Chemdogkm

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most medication has shelf life 1 year,not that it doesnt work after just that it is recomended to use it before
 

New Student

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Hello!!

I am new to all this and would liek to give this a try and learn more

Do I need a fume hood for this?

I will have a respirator and nice gloves, is there anything else I need to watch out for?

Thank you
 

William D.

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The main thing is to have time to cool the reaction while this does not get out of a flask with a volcanic effect. Evaporation that you can get the main IPA is not so critical.
 

New Student

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Thank you< so I probably don't need a fume hood for this
 

Chemdogkm

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depends on quantity of production,mostly just fumes, no open flames, dont ingest the poisonous chemicals.dont order chemicals from out of the country,they will get taken and maybe feds show up, dont talk to cops without a lawyer and dont let anyone in ur house unless they kick in the door with a warrant
 

Chemdogkm

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so i have an oily residue product,what is a good way to crystalize it?
 

golab071

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You need to use a solution of acid (phosphoric or sulfuric) in IPA. This is shown and explained in detail in the video available on the forum.
 

Chemdogkm

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After that.just takes forever to dry. So recrystalize with ethanol or xylene is what im thinkn
 

golab071

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Thank you for the previous responses.

The chemist has carried out their first (successful?) reaction and, as a result, has further questions.

The test subject, who evaluated the final product, compared it to the one commonly available on the street (according to police reports found online, its purity is usually around 10-20%).

I’d like to know whether the test subject had overly high expectations of the product, or if the inexperienced chemist might have made several mistakes during the process?

What can realistically be expected from the final product, and could further experiments significantly improve its quality?

The errors that, according to the chemist, may have affected the final product include:

• Completely skipping extraction with DCM (the chemist was prepared for it but lacked sufficient theoretical knowledge).

• Drying the product for too short a time and at too high a temperature.

Could this affect the product’s quality?

Does extraction with DCM involve adding DCM to the free base and collecting the appropriate layer? If so, are the layers clearly distinguishable, and which one (top/bottom) contains the product?

Could @G.Patton @William D. provide their input on this?
Thank you!
 

G.Patton

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Hello.
It is quite subjective, has he checked its melting point? Isomer ratio also play role in the product activity. In addition, there is direct dependence between its purity and potency.

It's hard to estimate its quality in accordance with your description. You should check its purity in laboratory (such as EnergyControl or so) and then try to find a problem. Is your product absolutely white?

this step is quite important in order to increase the reaction yield and get rid of Hg salts in final product.

It also can influence on the product quality in case of air exposure during its strong heating.

Yes, he has to add DCM to the reaction mixture stir it well and then separate layers. DCM layer is clearly be determinated by its transparency and smell.

By the way, will you sell your product here?
 

golab071

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Thank you!


No measurements were made, and the product was not 100% pure.


After adding the sodium hydroxide solution to the mixture, an oily layer separated after some time. So, should DCM be added to it after separation, or already at the stage of adding sodium hydroxide? I’m an amateur with a new hobby :) As you can see, I still have a lot to learn. I’ll follow the instructions and keep you updated on the progress. Any sale at this point is out of the question.
 

G.Patton

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>So, should DCM be added to it after separation, or already at the stage of adding sodium hydroxide?

It has to be added after NaOH aq sln addition and 5-10min stirring in order to let it reacts.
 
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