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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Consider

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Boss can I use alphamethylphenethylamine (amphetamine) from this reaction in replacement to ephedrine to synthesis methamphetamine using iodine and hypophosphorous acid, please
 

HEISENBERG

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Rose - the product is overoxidized (part of the amphetamine salt, due to the overuse of acid, turned into decomposition products and colored the rest of the powder).
Yellow - the product is not oxidized (due to a lack of acid, not all of the base was converted into salt, and its residues colored the rest of the powder).
Red - phenyl nitropropene did not react completely on amalgam, the reaction mixture was alkalized and acidified into salt, giving this color.
Green - mercury salts are contaminated with other metals, which result in color. In addition, it affects the formation of amalgam.
Brown - formation of resins during synthesis.

Study this thread http://chemforum.info/index.php?threads/amphetamine-assessment-protocol.349/
 
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RWG13

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Hello. I tried to do these synthesis, i got it done only on the third try, but with extremely small yield. From 10g of P2NP only ~0,5 of amphetamine phosphate.
Here are some possible reasons:
1. When I add a solution (10p2np, 100 ipa, 50 glacial acid) to amalgam, reaction begins immediately, and very intense. I cool it (without overcooling) and after this the reaction continues for about 4-5 minutes (with active release of heat) after which it begins to slowly subside, I tried to start it again using hot water, but the reaction does not start again, it slowly subsides. Please tell me if I made any mistake at this stage.
2. I also noticed a strange thing at the alkali stage. (I used a pipe cleaner that only listed sodium hydroxide). I added gradually (literally drop by drop), after I added half and started stirring, the solution became like wet gray sand, I already thought that everything was ruined again, and I added the remaining half and suddenly the mixture became liquid again. after which a transparent cloudy layer with a volume of 2.5 ml formed on top of it. I removed the top layer with a syringe, placed it in a separate container and ordered a 1:9 solution of isopropyl alcohol and 85% orthophosphate acid. The mass began to gather in white lumps, and at first it seemed that there were 3-4 grams, but after drying it turned out that there were 0.5 grams. What could I have done wrong? I would be very grateful for your help.
 

RWG13

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Resolved.
All problem was in alkalization process. I used a dry pipe cleaner in which only NaOH was indicated in the components. And so I weighed it as pure caustic soda. Although, as it turned out, in these mixtures NaOH is only 25-60% (I did not find the exact amount and other components too). In this case, it was decided to make a little more solution and add powder to it until it stops dissolving. I added the solution, removed the oil (so as not to spoil it with alkali if something happened) and added more alkaline solution, after which an oil layer formed again. For greater convenience, I also tried extracting the oil layer using Coleman fuel, the result was positive. The acidification process, in my opinion, is more convenient when the base is dissolved in something. The yield was 65-70% after washing with acetone and subsequent drying.
 

JohnWebb

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Guys, can I ask, is this normal?
After alkalinization I have 3 layers. In previous attempts, I've only ever had 2 layers

HsXu9jDfmz
 
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handle

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Top layer is the layer you want... bro...
 

9-Tryptophan

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"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."



Can I evaporate the solvent slowly on a hotplate at 100°? I know normally it should be vacuum distilled but my vacuum source is broken.
 

Johnson212

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I am a newbie, can I make mercury sulfate myself? How can I get mercury?
 

handle

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Easiest for me is to buy these mercury tilt switches $0.80c each.
KlxnUfktcJ
 

blockchain

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Can i use acetic acid (80%) If i dont have H2SO4?
 

Woody

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No
 

RWG13

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Yes, but check how to produce amphetamine acetate. And in any way you will have some loses in yield because of 20% of water in your acetic acid solution.
Probably you need to mix 1 ml of acetic acid to 10 ml of IPA, and try to add these solution, drop by drop and see any changes. And how I remember, acetate is not a white powder, but yellow “caramel”
 

Consider

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Please is phamethylphenethylamine (amphetamine) the same as ephedrine ?. can I use alphamethylphenethylamine (amphetamine) from this reaction in replacement to ephedrine to synthesis methamphetamine using iodine and hypophosphorous acid method
 

Consider

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Please can I used these amphetamine in replacement for ephedrine in iodine and hypophosphorous reaction to produce methamphetamine.
 

Consider

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Please can I use
 

lemon

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No. Just do methylation with formaldehyde in Al/Hg, it's very good route, you can go from d-amph.
 

magnesium_sulphate

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Can sulfuric acid be replaced by a 97% purity containing drain cleaner?
 

spongebomb

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when the drain cleaner is, 97% sulfuric acid, why not
 

handle

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When salting out the salt, it didn't turn white? Stayed clear and thickened to a Ph6. Why could this be?
 
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