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Synthesis of amphetamine[Video]

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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%.

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