Ich habe versucht, P2P aus P2NP mit Zinnchlorid-Dihydrat zu synthetisieren. Nach dem Abschrecken mit Wasser erhielt ich ein organisches gelbes Öl. Nach Zugabe von dcm bildete sich ein trübes, blassgelbes Gemisch aus dcm und p2p. Ich habe dem Gemisch Methylamin zugesetzt und dann Aluminium und HCl hinzugefügt, um es zu einer methamphetaminfreien Base zu reduzieren, und dann HCl-Gas hineingeleitet. Ich habe kein Quecksilberamalgam gebildet, da es verwendet wird, um die Bildung einer oxidativen Schicht über dem Aluminium zu verhindern, sondern ich habe die Reduktion mit Aluminium und HCl durchgeführt. Die Reaktion wurde durch den Schritt, bei dem ich dcm zugegeben habe, durcheinander gebracht.
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Question P2P-Synthese und Umwandlung in Meth
- Thread starter Zeus the chemist
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So, upon quenching with h20 did you thro it into a separatory funnel to remove h20 thus separating the aqueous from organic p2p/dcm layers?
To get anything of quality you would then distill your p2p layer to get a light yellow to pale clear liquid which smells like "burnt roses" but sweeter. Then you would want to figur out how much of each reagent solvent etc is necesary for a successful reaction calculating how many mols of each is required.
Once thats completed in a separate flask you'd combine the methylamine solution, catalytic amout of an acid, with the now freshly distilled p2p in. An IPA solution or similar alcohol. Cap it and set it aside allowing imine formation which is paramount for success.
While waiting for the imine, prepare your aluminum/mercury amalgum using mercuric chloride, nitrate, etc. H20 and aluminum making sure you add enough HgCl2 to ensure total amalgamation of the aluminum metal as too little really fucks your day up. Once your amalgum is "activated" dump the mercuric h20 and rinse your amalgum 2 more times with distilled h20. I say distilled because it will "grab" more mercury salts being that it is much less saturated woth minerals etc than tap water.
After rinsing set your preferentially 2 necked RBF up for overhead stirring in the center neck and a reflux condensor on the side neck with ice cold h20 flowing through the condesor. Make sure its ling enough as well 300mm is my go-to. While magnetic stirring is possible it's rather impractical during the first half of the reaction of the amalgum. Remember you want everything smashing into eachother so the molecules react fully.
To your amalgum begin the addition of your p2p/ipa/methylamine/acid solution. Your RM will begin increasing in temp however, the temp change is exteemely manageable and not anything that will flood your condensor like when making amphetamine using p2np with this method.
Upon the addition of your p2p solution to the amalgum prepare approx 200ml of 25% NaOH solution placing in your refrigerator or allowing cooling to ambient temps if no fridge. [I usually also include non iodized salt approx 10gr-15gr into my 25% NaOH solution to help with separation of the product from the amalgum once reaction has run to completion]
Allow contents to react for several hours to completion. Generally you can tell when it has completed by stopping the stirring an observing cessation of hydrogen bubbles while your rm becomes a more homogenous mixture than you began with. The RM will be a dark grey color and need to be quenched with by the earlier mentioned 25% NaOH/NaCl solution prepared and cooled earlier. Turn your stirrer back on and add in the Naoh/Nacl solution to your reaction vessel. You can remove the condensor and allow the contents to vent while becoming basified. This gets rid of excess methylamine gas in your rm. Allow your rm to stir another hour or 2. The NaOH destroys the left over aluminum metal to a degree and basifies the rm contents allowing for extraction using a non polar solvent once finished stirring.
Afterwards you need to extract your rm with a non polar solvent then workup as usual.
I'm just unsure as to your procedure which would be better written in detail to help
To get anything of quality you would then distill your p2p layer to get a light yellow to pale clear liquid which smells like "burnt roses" but sweeter. Then you would want to figur out how much of each reagent solvent etc is necesary for a successful reaction calculating how many mols of each is required.
Once thats completed in a separate flask you'd combine the methylamine solution, catalytic amout of an acid, with the now freshly distilled p2p in. An IPA solution or similar alcohol. Cap it and set it aside allowing imine formation which is paramount for success.
While waiting for the imine, prepare your aluminum/mercury amalgum using mercuric chloride, nitrate, etc. H20 and aluminum making sure you add enough HgCl2 to ensure total amalgamation of the aluminum metal as too little really fucks your day up. Once your amalgum is "activated" dump the mercuric h20 and rinse your amalgum 2 more times with distilled h20. I say distilled because it will "grab" more mercury salts being that it is much less saturated woth minerals etc than tap water.
After rinsing set your preferentially 2 necked RBF up for overhead stirring in the center neck and a reflux condensor on the side neck with ice cold h20 flowing through the condesor. Make sure its ling enough as well 300mm is my go-to. While magnetic stirring is possible it's rather impractical during the first half of the reaction of the amalgum. Remember you want everything smashing into eachother so the molecules react fully.
To your amalgum begin the addition of your p2p/ipa/methylamine/acid solution. Your RM will begin increasing in temp however, the temp change is exteemely manageable and not anything that will flood your condensor like when making amphetamine using p2np with this method.
Upon the addition of your p2p solution to the amalgum prepare approx 200ml of 25% NaOH solution placing in your refrigerator or allowing cooling to ambient temps if no fridge. [I usually also include non iodized salt approx 10gr-15gr into my 25% NaOH solution to help with separation of the product from the amalgum once reaction has run to completion]
Allow contents to react for several hours to completion. Generally you can tell when it has completed by stopping the stirring an observing cessation of hydrogen bubbles while your rm becomes a more homogenous mixture than you began with. The RM will be a dark grey color and need to be quenched with by the earlier mentioned 25% NaOH/NaCl solution prepared and cooled earlier. Turn your stirrer back on and add in the Naoh/Nacl solution to your reaction vessel. You can remove the condensor and allow the contents to vent while becoming basified. This gets rid of excess methylamine gas in your rm. Allow your rm to stir another hour or 2. The NaOH destroys the left over aluminum metal to a degree and basifies the rm contents allowing for extraction using a non polar solvent once finished stirring.
Afterwards you need to extract your rm with a non polar solvent then workup as usual.
I'm just unsure as to your procedure which would be better written in detail to help
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