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

HIGGS BOSSON

Active member
Expert
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%.
 
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William Dampier

Active member
Expert
What do you think about using ethyl acetate instead of acetic acid to reduce phenylnitropropene?
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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rickyrick

Member
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.
 

William Dampier

Active member
Expert
Yes, overhead stirring, maybe. You can use plastic barrels for this reaction, using water cooling "barrel in barrel" system.
 
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William Dampier

Active member
Expert
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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HIGGS BOSSON

Active member
Expert
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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rickyrick

Member
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?
 

William Dampier

Active member
Expert
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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William Dampier

Active member
Expert
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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rickyrick

Member
U 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 u need polypropylene shaft or teflon coating
Any special type of plastic tubing that can handle the heat from reaction and cold/hot stress?Thank you sensei.
 

Xiaoyan

New member
what about the orange speed? i have a chemical recipe. supposedly the same products, but when precipitate is occurring, it came in pink color (during boiling) and orange when its cold.
anyone knows some about that?
 

HEISENBERG

Administrator
Staff member
ADMIN
what about the orange speed? i have a chemical recipe. supposedly the same products, but when precipitate is occurring, it came in pink color (during boiling) and orange when its cold.
anyone knows some about that?
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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Xiaoyan

New member
Wow... i have no words.
really thanks
im really interested in doing the synthesis, if i can found all i need.... ;P
do you have any advice for this amateur chemist?
first of all, thanks
 
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