Amphetamine synthesis from P2NP via Al/Hg (video)
- Thread starter HIGGS BOSSON
- Start date
They scale linearly, so half of everything.Reflux is not obligatory to happen for reaction to take place, if you control the reaction properly in an appropriate flask with a beefy condenser it won’t reach reflux even, especially aith 5g.If you reaction is not starting at all however with the addition of your propene, I would maybe check : if amalagam was done correctly, the purity of my raw materials (especially the propene).And ffs use distilled.
Normally, one does not dry concentrated sulfuric acid at all, but uses it to dry itself.
If I mix 1ml H2SO4 96% and 5ml dry IPA for titration, I have approx. 0.04ml water in the solution. In such a constillation I think there is no reason to use desiccant.
It will certainly not do any harm, but it is questionable whether it will work.
If I mix 1ml H2SO4 96% and 5ml dry IPA for titration, I have approx. 0.04ml water in the solution. In such a constillation I think there is no reason to use desiccant.
It will certainly not do any harm, but it is questionable whether it will work.
I've been having issues with PMK all/hg reduction, I have a large amount of unreacted aluminium leftover after a 240g ketone rxn. The vessel heated on its own with reflux to around 65c and dropped to 40c over the course of 90mins. Then heat was applied to bring it up to 50-60c for 3-4 hours.
Pie pans were used and cut into 1 cm small strips and 10% excess was added to osmium writeup. After basifying the ai was reduced. Then goods extracted with toluene and washed with naoh solution. I'm hoping for atleast 100g yeild. If not then I'm fucked and will have to save some more money for another rxn and just used foil so it gets eaten.
I recall there being maybe 50% ai leftover. This was 100% aluminium disposable baking pans. I waited about 45-60mins for amalgamation to start and only a few pieces were floating, I assumed its because its thicker ai..but there was bubbling going on the the solution had a silvery appearance.. It seemed ready. And the rxn heated to 65c on its own so I'm sure it was ready...maybe I just have to gas and see the yeild...I have a feeling it going to be bad lol. D
oes osmium already add extra aluminium? Maybe I added excess on excess lol. Anyways I think thick foil would be OK for 200-300g reduction. I wish I realized this and stuck with foil on these larger rxns...but this is how I learn. If the reaction went to 65c with Al pans then with foil it might be too exothermic right? So my Al thickness might be on point and maybe I have to let amalgamate longer until all pieces are floating? it seemed to me like it was going and exothermic reaction kicked in.
If been wasting quite a bit of material and time on trying to scale up and each time I'm playing around with thicker Al, when I think I should stick to maybe a thicker foil, that way it all gets consumed and the temps may go up to like 75c but can cool it to keep under 70 no problem. If I knew about the NMF route before preparing for osmium route then I would being using NMF and I think I'd have less problems.
I will report back with yeild on the pie pan run.
Pie pans were used and cut into 1 cm small strips and 10% excess was added to osmium writeup. After basifying the ai was reduced. Then goods extracted with toluene and washed with naoh solution. I'm hoping for atleast 100g yeild. If not then I'm fucked and will have to save some more money for another rxn and just used foil so it gets eaten.
I recall there being maybe 50% ai leftover. This was 100% aluminium disposable baking pans. I waited about 45-60mins for amalgamation to start and only a few pieces were floating, I assumed its because its thicker ai..but there was bubbling going on the the solution had a silvery appearance.. It seemed ready. And the rxn heated to 65c on its own so I'm sure it was ready...maybe I just have to gas and see the yeild...I have a feeling it going to be bad lol. D
oes osmium already add extra aluminium? Maybe I added excess on excess lol. Anyways I think thick foil would be OK for 200-300g reduction. I wish I realized this and stuck with foil on these larger rxns...but this is how I learn. If the reaction went to 65c with Al pans then with foil it might be too exothermic right? So my Al thickness might be on point and maybe I have to let amalgamate longer until all pieces are floating? it seemed to me like it was going and exothermic reaction kicked in.
If been wasting quite a bit of material and time on trying to scale up and each time I'm playing around with thicker Al, when I think I should stick to maybe a thicker foil, that way it all gets consumed and the temps may go up to like 75c but can cool it to keep under 70 no problem. If I knew about the NMF route before preparing for osmium route then I would being using NMF and I think I'd have less problems.
I will report back with yeild on the pie pan run.
Last edited:
IMO any Al thick foil is good depending on your scale. Store bought heavy duty foil for doing small scale and even bigger reactions but the All granules or Al fine CNC shavings looks nice.
I'm.not familiar with amphetamine but that could be your drying agent possibly. If its your yeild than it looks OK to me.
I'm.not familiar with amphetamine but that could be your drying agent possibly. If its your yeild than it looks OK to me.
When you taste the product at first, it will taste very salty, and in the end, amphetamine taste appears
Isopropanol is ok i presume ?
we rinse the ballon, and put the the result on the fine sieve for going with the rest before alkalinization ?
no need to evaporate isopropanol or something like that ?
(any idea of max isopropanol quantity we can use for the rinse?)
we rinse the ballon, and put the the result on the fine sieve for going with the rest before alkalinization ?
no need to evaporate isopropanol or something like that ?
(any idea of max isopropanol quantity we can use for the rinse?)It can be Sodium Sulphate... Your reaction might not have gone all the way through. I had the same issue in the beginning, had Na2SO4 as well and others. The solution was not to rinse the amalgam (just draining the water) and also my rule for the readiness is when all the Al comes up to the surface and you can also hear a sizzling sound. There are also small bubbles appearing. This is when I consider ithe amalgam ready, and this solved the lack of reaction problem. My yield varies usually only around 50%, but never had a non-reactive amalgam since then.
Excuse me . But we did not use sodium sulfate in this synthesis. What is its relationship to the topic? If you would allow, please explain to me more. I did not understand the idea. Thank you
Hi, I`m not an expert by any means, so others might confirm or correct this, but when you add sulphuric acid (H2SO4) to the mixture if there is no amphetamine base present (i.e. the reduction did not happen) then the SO4 might form a salt with the Sodium (Na). The Sodium is present in the solution from the NaOH added earlier.