Methamphetamine synthesis from P2P via Aluminum amalgam

[G.Patton]

Hello, yes
You have to get methylamine free base. Hydrochloric salt will not work.

 

[bndr]

Methylamine freebase is a gas, in this procedure he uses methylamine HCL, the sodium hydroxide freebases it as its added to the reaction. So yes Methylamine HCL can be used. Its all ive ever used....

 

[WilliamK]

We are not using pure methylamine but 25% solution which is dissolved in water.
In this form, it's obliviously a liquid

 

[Lordoftheshard 2]

500 Gms Aluminium Uncoated Metal Powder 100% Grade 420A Fine Powder FREE SHIP
It's uncoated.and that's what the Mercury does strips the coating off
Can I use this instead of foil and mercury chloride

 

[diogenes]

Sorry to say, but I don`t think this would work for several reasons. Hg does not facilitate the reduction by stripping the Aluminium oxide off (although it does destroy the coating in the process once it came in contact with the aluminium even at the tiniest spot). The reduction happens because Hg is more electropositive, which means that once a contact is made with the Al, Hg sucks the electrons out of the Aluminium, leading to the oxidation of Al into Al(OH)3 (the sludge you see in the reaction). It creates a bridge for electron transfer from the Aluminium to your product which is reduced (given electrons).

If there was no Hg the Aluminium would self-destroy in a very stormy way generating huge amounts of H2 in a flash. By the way this would happen any time if there was no Al2O3 protective layer as Al is very reactive and the oxide layer is the only reason Al can exist in air.

The Al powder would also have protective layer (Aluminium oxide - Al2O3) even on the tiny Al parts. The problem with powdered Al is that the reaction would happen all to quick, you would not be able to control it. Even when your foil is too thin, it becomes quite problematic if not impossible to prevent the aluminium from being consumed before your product gets reduced. Imagine this with the powdered form, it would just it itself up almost instantly.

 

[Lordoftheshard 2]

Thank you much appreciated now on the hunt for mercury chloride

 

[OrgUnikum]

No need for HgCl2 in special, any mercury salt works, the nitrate even better then HgCl2 which is just the most common and working very well.

Metallic mercury can be used too, just if you happen to find some old thermometers or mercury electric switches which were common in cars or also in chest freezers where they switched on the light when the lid was raised.
Mercury metal is easily transformed into HgCl2, all whats needed is some nitrate salt, anyone works and only a tiny amount is needed to catalyze this reaction which works like this: Mercury metal into a vessel, cover it with HCl, 30% is fine. You can add some alcohol to have the mercury well covered. Then add a knifes tip of any nitrate you can get, all work. Warm it up a bt if the reaction is sluggish, do this in a well ventilated place.
On addition of the nitrate the reaction starts and it works like this: The HCl will replace the nitric acid in the nitrate and there is suddenly free nitric acid. Nitric acid attacks mercury and forms mercury nitrate which due to the HCl present is turned into HgCl and HgCl2.You can use this soup directly for amalgamation of the Aluminium,use some more as usual as some will react with the excess HCl, thats no problem.

 

[Ortist]

HCl will not replace nitric in Hg nitrate as nitric is stronger than HCl. If I understood you right . You either have to react metallic mercury with nitric acid to get a nitrate and use it as is or get a nitrate, then basify it with NaOH to get a mercury oxide (precipitates) then react the oxide with HCl. Another option which I used is to make Hg acetate (Hg+Acetic acid+H2O2) -> white precipitate, then add HCl uuntil precipitate disappears and use this soup for amalgamation.

 

[OrgUnikum]

Mercury + diluted nitric acid as formed by HCl and a nitrate salt (you WILL have some nitric acid due to the dissociation and equilibrium and such crap) -> mercury(I)nitrate. Reacting mercury(I)nitrate with HCl is one of the common ways to get HgCl2.

In the end the proof is always in the pudding: Just try it. It works.

There was some headscratching back then 20 years ago when Polverone brought this up at sciencemadness.org, but as he actually tried it before posting, and nobody doubted this, well, he is known and respected and he owns the board ....
.... over time heaps of people have used the method, also I am recommending it often since it was posted over 20 years ago and nobody came to rip off my head in all this time....

all good, no worries
/ORG

 

[Ortist]

This writeup is a total mess. Following it as is will give you 10% yeld. Or may be less.

1. Aluminium amalgam must be prepared in advance, it is important step
2. Add your p2p, Methylamine to amalgam along with isopropanol
3. Keep reaction temp <30 degrees
4. With 40g of p2p and 40g aluminium FOIL you'll get 100% runaway .
5. Add NaOH/KOH before filtering Al/Hg sludge, it makes filtering process easier and kills remaining Al
6. And so on...

 

[Jordan Belfort]

I did before on 200L drums, 100L drums are also fine, and did one pot reaction.

350-400 grams of mercury on 10L b (400 grams is really a lot aggressive), 15L methylamine 40% and then like 30L methanol.
The foil I am unsure, I had in the end made like 2/3 of a bucket full with scrathed/damaged foil (no balls) so it was that weight.

In the end it was to much foil.
Yield; 12L at PH 12.

Back then with methylamine, everyone knows there are better alternatives for that when working with, f.e., with Al/Hg

 

[Jordan Belfort]

Use thick foil, and yes it's exthrothermic. It wasn't kilos was 2/3 of a 30L bucket.

Try use thick foil. But with they mono ratio it was good although i would suggest nitromethane instead of methalamine and destill and reuse all.

 

[OrgUnikum]

In big batches you drip in the Ketone (P2P) as fast as possible without the reaction jumping out of the flask/blowing through the condenser. A huge excess of methylamine* must be used as P2P forms the Imine not as willingly like MDP2P for example. Stirring is essential for decent yields in bigger batches. Use Al-granules about 2mm size 99,99xx% purity not foil. The amalgam can be prepared in situ, in the reaction vessel, use a generous amount of HgCl2 and warm it up to 30 °C to get this going cover the Al with alcohol + 20% water. Amalgamation works better with water added.

*4 molar or more. That's about the same weight Methylamine as P2P, more MeNH2 is better, you can recover it easily when the reaction is finished and re-use it. A efficient condenser is needed not to blow out too much methylamine with the refluxing reaction. Alternatively the top of the condenser can be connected with a tube to a vessel with water or better alcohol where the MeNH2 is collected, this avoids the horrible Amine stink too.
Ethanol (denaturated is fine) gave best results. When all P2P was added the reaction is stirred and heated to reflux until all Al is consumed. It is simple: The longer you run it the better is the yield. After finishing adding the Ketone 4 hours are absolute minimum, 5 hours are a good compromise, 12 hours improve the yields compared to 8 hours only by about 5%, longer is nonsense.

At 30 °C the reaction would have to run for days, 60 hours minimum but maybe it takes a week.
Al granules are much better and the reaction can be refluxed no problem.
Adding al P2P immediately is calling for disaster and simply retarded, why would anybody want to do this? You run it in as fast as possible, it offers perfect control, you see how far the reflux goes up the condenser and when it comes to 1/3rd you stop and wait until it calms down. Good mechanical stirring is a must have or the reaction is uncontrollable (pockets of Ketone form and react all of a sudden).

Yields are never as good as with MDP2P but with a lot of Methylamine and running it 8 hours + over 80% yield can be achieved.

Workup is adding Hydroxide and lots of water the distilling alcohol/methylamine and then the rest alcohol out of the vessel, add more water and steamdistill slowly - meth steams over very easily no need to push it, quality is much better this way. The oil from the steamdistillation can be turned into the salt directly if one did not push it, but of course further cleanup steps are always improving purity, well its up to you if you want to take pride in your product or actually do not give a fuck as its for money and for the money alone.

 

[Lordoftheshard 2]

Reflux temp.50c is this correct as my friend told.me.this also.when dripping in the p2p he said don't let the reaction mix go above 50c and slow the drip rate down if does

 

[OrgUnikum]

Reflux temperature is when it boils and thats depending on the boiling point of the mixture what means with a lot of methylamine in there it will be about 45 to 50 °C as thats when the water/alcohol/methylamine azeotrope boils. You cannot get it hotter without a pressure vessel. Problem is methylamine escaping, I already told how to solve this problem by catching and re-using the MeNH2 which boils off. At lower temperatures you wwill still have MeNH2 loss but also the reaction will take forever and a day or two or five.

 

[Lordoftheshard 2]

So what do you recommend ratios and so forth to do the synthesis in 8h it say 2on here with the ratios provided here is rather reflux it for 8h to do the job properly

 

[xile]

one has a question about mercury chloride. Could one make that using elemental mercury and hydrochloric acid? Hg + 2 HCl -> HgCl2 + H2 ? Is this reaction realistic? How much mercury is in a clinical thermometer?

 

[Ortist]

No this is unrealistic. What you can do if you need a chloride:

1. Take metallic mercury in a beaker (from a termometer)
2. Add 5ml of glacial acetic acid and 5ml of hydrogen peroxide (30..50%)
3. Stir until all mercury turns into white powder
4. Slowly add hydrochloric until clear solution is obtained
5. Carefully evaporate until syrup and cool

Another option is to make nitrate with nitric acid, then basify to make an Hg oxide, then dissolve in HCl. This method generates alot of fumes because of nitric acid

Another option which I didn't try is to react Hg with 50/50 mixture of HCl and H2O2 with stirring. MAYBE it will work. Acetate->Chloride works very well

 

[xile]

This way is realistic?
Hg + 2HCl + H2O2 → HgCl2 + 2H2O

 

[Ortist]

you can try. it is exotermic so beaker need to be cooled or h2o2 will decompose.
but
Hg+Acetic+H2O2 -> Hg.Acetate
Hg.Acetate + HCl -> HgHl2

Is proven to work, it is quick, and no smell

 

[OrgUnikum]

In this case it is necessary to point out that one better does not attempt to dry HgCl2 on a hotplate or even just by having it stand on air as HgCl2's alchemist name is "corrosive sublimate" and that says everything, this salt sublimates easily, say it goes from solid into the air without going through the liquid state. So when attempting to dry HgCl2 without professional equipment one will get a lot of it in the air and inhaling mercury or its salts is one of the sure and really bad ways to get mercury poisoning of the worst kind. Also keep all containers closed all the time and open only for retrieving and directly using the needed amount.

 

[Ortist]

Yes thats true. Thats why I said "cafrefully evaporate". And of course it is must not be done in a closed room. Without professional equipment it is better done with all windows open and a fan blowing vapours straight to the window. Or just stick to nitrate salt.

However I usually evaporated it until syrup and then diluted it with big amount of water to make an amalgamation solution. It is safer to store and easier to dose.

 

[OrgUnikum]

You need to add a small amount of a nitrate like salpeter or ammonium nitrate or potassium nitrate or silver nitrate (thats sold for analytical reasons by every chemistry shop in small amounts but you need only a tiny amount like a pointed knifes tip to catalyze the reaction).
I posted the mechanism how it works just before.
The old style clinical thermometers had a gram or so of mercury, switches have often five gram or more, as Ebay and Amazon have banned the sale of anything with mercury (where I live at least) your best bet are classifieds.

 

[Win Win]

Hi sir. May i know your reflux for two hour is room temperature reaction or need to warm up? Section 2

 

[Win Win]

Hi sir
your reflux 2 hour is room temperature reflux or need heat up temperature?

 

[Win Win]

Can ether change to EA?