Step 1: Prepare the phenylnitropropene solution.
Weigh 5 grams of phenylnitropropene and mix with 50 ml of isopropyl alcohol in a beaker until completely dissolved.
Then add 25 ml of glacial acetic acid and mix until homogeneous.
Step 2: Preparation of mercuric nitrate.
a) If you have mercuric nitrate, simply measure 50...100 mg for the reaction and add it after the water
step 3 Aluminum from which the foil is made must be activated for the reduction reaction. Aluminum is activated with mercury nitrate. The goal is to remove the oxide layer from the surface of the foil and not allow the mercury nitrate to completely react with the foil. Readiness is determined visually using indicators. The foil becomes completely dull and a large number of small hydrogen bubbles are released. At the moment when a precipitate begins to form at the bottom, it is necessary to drain the liquid so that the foil remains in the flask. Rinse the foil from the remaining mercury nitrate with a fresh portion of water. Drain the water again and leave the foil in the bottle.
step4 Add the phenylnitropropene solution to the flask with the prepared amalgam and place the reflux condenser on the flask. Start stirring the reaction mixture with gentle circular movements. The reaction mass begins to heat up (exothermic reaction). It is important to maintain the temperature at ~60ºC and not allow the reaction to freeze. The temperature is controlled by cooling. Sometimes an inverted refrigerator connected to running water is sufficient, but more often it is necessary to place the flask in a small tub of cold water (ice or snow). To prevent the reaction from freezing, it should be cooled quickly by immersing the flask in water and then immediately removing it. If the temperature is still high and the reaction mixture continues to rise, the cooling procedure should be repeated. Cool carefully, there is a possibility that the reaction will be stopped by excessive cooling. After the violent part of the reaction is over, the flask can be placed on the surface and stirred from time to time until the bubbling stops completely.
now 5 Dissolve 25 g of NaOH in 75 ml of water in a beaker. Dissolution is accompanied by strong heating of the liquid. Therefore, this procedure is performed in advance so that the solution cools down in due time. It is not recommended to use a hot solution.
When the reaction stops and there are no traces of reaction in the flask, add the caustic solution. It is dangerous to add the entire volume of lye at once, since the entire reaction mixture can solidify. Add 1/5 of the total volume, mix well, wait for the foam to subside, and then add more. After adding the lye, mix well and pour into a glass. Wait 30 ... 60 minutes for the mixture to break up. Wait for the clear boundaries of the layers and select the top layer. It is usually transparent, but sometimes it is yellowish.
step7 Add 10 ml of acetone to 1 ml of concentrated sulfuric acid, stir and begin acidification. Add a drop of sulfuric acid solution to the oil until the pH is 6. Use pH paper to measure the pH. Each drop will contain flakes, this is amphetamine sulfate. The result of acidification should be a mixture similar to sour cream. After acidification, the mixture should be placed in the freezer for 2-4 hours to precipitate. This "sour cream" must be filtered and dried. A dense cloth, paper filter or vacuum filtration device can be used as a filter.
is this order correct?
Weigh 5 grams of phenylnitropropene and mix with 50 ml of isopropyl alcohol in a beaker until completely dissolved.
Then add 25 ml of glacial acetic acid and mix until homogeneous.
Step 2: Preparation of mercuric nitrate.
a) If you have mercuric nitrate, simply measure 50...100 mg for the reaction and add it after the water
step 3 Aluminum from which the foil is made must be activated for the reduction reaction. Aluminum is activated with mercury nitrate. The goal is to remove the oxide layer from the surface of the foil and not allow the mercury nitrate to completely react with the foil. Readiness is determined visually using indicators. The foil becomes completely dull and a large number of small hydrogen bubbles are released. At the moment when a precipitate begins to form at the bottom, it is necessary to drain the liquid so that the foil remains in the flask. Rinse the foil from the remaining mercury nitrate with a fresh portion of water. Drain the water again and leave the foil in the bottle.
step4 Add the phenylnitropropene solution to the flask with the prepared amalgam and place the reflux condenser on the flask. Start stirring the reaction mixture with gentle circular movements. The reaction mass begins to heat up (exothermic reaction). It is important to maintain the temperature at ~60ºC and not allow the reaction to freeze. The temperature is controlled by cooling. Sometimes an inverted refrigerator connected to running water is sufficient, but more often it is necessary to place the flask in a small tub of cold water (ice or snow). To prevent the reaction from freezing, it should be cooled quickly by immersing the flask in water and then immediately removing it. If the temperature is still high and the reaction mixture continues to rise, the cooling procedure should be repeated. Cool carefully, there is a possibility that the reaction will be stopped by excessive cooling. After the violent part of the reaction is over, the flask can be placed on the surface and stirred from time to time until the bubbling stops completely.
now 5 Dissolve 25 g of NaOH in 75 ml of water in a beaker. Dissolution is accompanied by strong heating of the liquid. Therefore, this procedure is performed in advance so that the solution cools down in due time. It is not recommended to use a hot solution.
When the reaction stops and there are no traces of reaction in the flask, add the caustic solution. It is dangerous to add the entire volume of lye at once, since the entire reaction mixture can solidify. Add 1/5 of the total volume, mix well, wait for the foam to subside, and then add more. After adding the lye, mix well and pour into a glass. Wait 30 ... 60 minutes for the mixture to break up. Wait for the clear boundaries of the layers and select the top layer. It is usually transparent, but sometimes it is yellowish.
step7 Add 10 ml of acetone to 1 ml of concentrated sulfuric acid, stir and begin acidification. Add a drop of sulfuric acid solution to the oil until the pH is 6. Use pH paper to measure the pH. Each drop will contain flakes, this is amphetamine sulfate. The result of acidification should be a mixture similar to sour cream. After acidification, the mixture should be placed in the freezer for 2-4 hours to precipitate. This "sour cream" must be filtered and dried. A dense cloth, paper filter or vacuum filtration device can be used as a filter.
is this order correct?
- By golab071
This protocol is not complete, but it should work. The step of extracting the free base is missing, which is crucial for obtaining a higher quality and purity product. This also minimizes the risk of mercury poisoning, as mercury is toxic. I am also not sure if this amount of NaOH will be sufficient—add the solution until the pH reaches 11.
