What's the exact process of making the P2NP+IPA+GAA solution? Is it just mixing the appropriate quantity of each compound in a beaker, stirring it a bit and then letting it cool? I'm not sure why this part was skipped from the video.
Al/Hg aracılığıyla P2NP'den amfetamin sentezi (video)
- Thread starter HIGGS BOSSON
- Start date
so i have an oily residue product,what is a good way to crystalize it?
Thank you for the previous responses.
The chemist has carried out their first (successful?) reaction and, as a result, has further questions.
The test subject, who evaluated the final product, compared it to the one commonly available on the street (according to police reports found online, its purity is usually around 10-20%).
I’d like to know whether the test subject had overly high expectations of the product, or if the inexperienced chemist might have made several mistakes during the process?
What can realistically be expected from the final product, and could further experiments significantly improve its quality?
The errors that, according to the chemist, may have affected the final product include:
• Completely skipping extraction with DCM (the chemist was prepared for it but lacked sufficient theoretical knowledge).
• Drying the product for too short a time and at too high a temperature.
Could this affect the product’s quality?
Does extraction with DCM involve adding DCM to the free base and collecting the appropriate layer? If so, are the layers clearly distinguishable, and which one (top/bottom) contains the product?
Could @G.Patton @William D. provide their input on this?
Thank you!
The chemist has carried out their first (successful?) reaction and, as a result, has further questions.
The test subject, who evaluated the final product, compared it to the one commonly available on the street (according to police reports found online, its purity is usually around 10-20%).
I’d like to know whether the test subject had overly high expectations of the product, or if the inexperienced chemist might have made several mistakes during the process?
What can realistically be expected from the final product, and could further experiments significantly improve its quality?
The errors that, according to the chemist, may have affected the final product include:
• Completely skipping extraction with DCM (the chemist was prepared for it but lacked sufficient theoretical knowledge).
• Drying the product for too short a time and at too high a temperature.
Could this affect the product’s quality?
Does extraction with DCM involve adding DCM to the free base and collecting the appropriate layer? If so, are the layers clearly distinguishable, and which one (top/bottom) contains the product?
Could @G.Patton @William D. provide their input on this?
Thank you!
- By G.Patton
Hello.
It is quite subjective, has he checked its melting point? Isomer ratio also play role in the product activity. In addition, there is direct dependence between its purity and potency.
It's hard to estimate its quality in accordance with your description. You should check its purity in laboratory (such as EnergyControl or so) and then try to find a problem. Is your product absolutely white?
this step is quite important in order to increase the reaction yield and get rid of Hg salts in final product.
It also can influence on the product quality in case of air exposure during its strong heating.
Yes, he has to add DCM to the reaction mixture stir it well and then separate layers. DCM layer is clearly be determinated by its transparency and smell.
By the way, will you sell your product here?
It is quite subjective, has he checked its melting point? Isomer ratio also play role in the product activity. In addition, there is direct dependence between its purity and potency.
It's hard to estimate its quality in accordance with your description. You should check its purity in laboratory (such as EnergyControl or so) and then try to find a problem. Is your product absolutely white?
this step is quite important in order to increase the reaction yield and get rid of Hg salts in final product.
It also can influence on the product quality in case of air exposure during its strong heating.
Yes, he has to add DCM to the reaction mixture stir it well and then separate layers. DCM layer is clearly be determinated by its transparency and smell.
By the way, will you sell your product here?
- By golab071
Thank you!
No measurements were made, and the product was not 100% pure.
After adding the sodium hydroxide solution to the mixture, an oily layer separated after some time. So, should DCM be added to it after separation, or already at the stage of adding sodium hydroxide? I’m an amateur with a new hobby
As you can see, I still have a lot to learn. I’ll follow the instructions and keep you updated on the progress. Any sale at this point is out of the question.
No measurements were made, and the product was not 100% pure.
After adding the sodium hydroxide solution to the mixture, an oily layer separated after some time. So, should DCM be added to it after separation, or already at the stage of adding sodium hydroxide? I’m an amateur with a new hobby
As you can see, I still have a lot to learn. I’ll follow the instructions and keep you updated on the progress. Any sale at this point is out of the question.Can I substitute DCM for Acetone in Amphetamine Synthesis?
Hey fellow chemists!
I'm currently working through an amphetamine synthesis protocol (thanks to Amine expert guidance) and I'm curious about substituting dichloromethane (DCM) for acetone. Specifically, I'm wondering if it's possible to use DCM as a replacement in the following steps:
Thanks for sharing your experiences and expertise!
Hey fellow chemists!
I'm currently working through an amphetamine synthesis protocol (thanks to Amine expert guidance) and I'm curious about substituting dichloromethane (DCM) for acetone. Specifically, I'm wondering if it's possible to use DCM as a replacement in the following steps:
- Work-up: after extracting with DCM, could I use it again to wash the organic layer instead of acetone?
Thanks for sharing your experiences and expertise!
Last edited:
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.