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Amphetamine synthesis from P2NP via Al/Hg (video)
- Thread starter HIGGS BOSSON
- Start date
In the video synthesis of amphetamine, reagents are used:
Description of amphetamine synthesis video.
- 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;
- 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%.
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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@HIGGS BOSSON in the second video they say 0.1g of Mercury (II) nitrate and in your write up 0.3g what is the correct one?
It can be used, especially technical grade ethyl acetate because it contains alcohol and acetic acid if it was not additionally purified in production.
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Hi,is it viable to scale it up?What kind of reaction vessel would be needed to handle the exothermic reaction and what kind of condenser?overhead stirring maybe?Means of cooling?You are a boss for this video tho.Thanks.
Yes, overhead stirring, maybe. You can use plastic barrels for this reaction, using water cooling "barrel in barrel" system.
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Does it need reflux condenser then?Or sealed hermeticaly?Pressure release of some kind?Thank you very much for your answer.
Without a reflux condenser, we will deal with the evaporation of alcohol. If the precipitate turns into a stone, add pure alcohol to the reaction again. Fully sealed barrel is not suitable, as we will deal with strongly increasing pressure
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Unfortunately, this reaction scales with a loss in yields. Optimally, I was able to load 100 g of phenyl nitro propene in a 20 L flask, with cooling in a basin with ice water, the solution of p2np in amalgam was added in 3 portions.
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thanks for your answers guys.What amount of P2NP would be able to get reacted in a 200l barrel with good cooling and constant overhead stirring?Do you think it is viable due to loss in yields?
Max quantity what I know was 2,5 kg P2NP per this reaction, but need good control for temperature. Gradual scaling of the reaction - the best choice. With any problems with scaling, it is better to solve them on smaller quantities. We can help on this path, with feedback.
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You can use radiant floor tubing and cold water for chilling. Tubes twist the spirals inside the barrel and let the flowing cold water, when necessary. And when necessary, let the hot water for heating. Plastic tube does not react with mixture. For overhead stirrer, you need polypropylene shaft or teflon coating
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Any special type of plastic tubing that can handle the heat from reaction and cold/hot stress?Thank you sensei.
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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/
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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- By RWG13
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.
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.
- By RWG13
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.
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.
- By Codoi
Is there any difference in potency betwen this method and cucl2+nabh4?
I have recived a batch of speed (1 line and you can t sleep 24 hours+grinding teet,also a verry different smell than the one i cooked myself with the cucl2 method(verry clean in my oppinion.)
Could the first one contain residues from the synthesis or something?thus the different smell and effect(i m atraching a photo with both ,mayb
e it helps)
I have recived a batch of speed (1 line and you can t sleep 24 hours+grinding teet,also a verry different smell than the one i cooked myself with the cucl2 method(verry clean in my oppinion.)
Could the first one contain residues from the synthesis or something?thus the different smell and effect(i m atraching a photo with both ,mayb
e it helps)