amalgamation problems

[CharmingKid]

Hi everyone,

So I have a problem with the Al/Hg amalgamation. I tried it a few times and I don’t know what I am doing wrong and I did it on smaller scales (10 ml PMK)- after amalgamation started (indicated by formation of small bubbles and gray water) I added the methylamine and the PMK and it seems like something happened- because the temperature rose to 50 Celsius degrees but then it stuck there for approximately hour and then cooled down to room temperature and all the aluminum foil disappered

Any thoughts?

 

[G.Patton]

Hello, what is a problem? http://bbzzzsvqcrqtki6umym6itiixfhn...mphetamine-from-p2p-via-aluminum-amalgam.184/

 

[CharmingKid]

HI,
The problem is that apparently the reaction is not happening and I a not sure why- the reaction suppose to take much longer and get much hotter

 

[UWe9o12jkied91d]

Are you weighing your salts? Dare I ask are you weighing you alu?If proportions are correct amalgamation is gentle until all of the aluminium floats then it gets going.If yours is violent to begin with it's too little salts in fact.
If everything here is good then maybe try only rinsing once.Also you might be overcooling at the first sight of thermal expansion.Temp of water used can be increased a bit if youre using cold

 

[G.Patton]

It is quite hard to understand your problem without pictures. You think that reaction doesn't happened but you don't have any proof, right? Have you read my post? You need to boil your reaction mixture after self-heating.

 

[CharmingKid]

Yes, I weight the aluminom foil and the mercury (in my case I have mercury dichloride). I don't think the amalgamation is too violent and I think that I have the right proportion- 20 grams of aluminum foil and 0.1 gram HgCl2 , but I will try again with hotter water and one rinsing.

 

[CharmingKid]

I read your post- but the post is for methamphetamine synthesis and I need MDMA synthesis but I will try to boil my reaction mixture next time

 

[G.Patton]

I think it's to small. I think 0.3-0.35 is ok. http://bbzzzsvqcrqtki6umym6itiixfhn...threads/aluminium-amalgam-al-hg-summary.1271/
Sorry, my mistake. I thought we are talking about p2p->meth.

 

[UWe9o12jkied91d]

you need circa 0.1g / 12g ish alu

 

[CharmingKid]

So I tried again several times and I think the amalgamation worked well, but then I extracted the reaction mixture with NaOH and isopropanol- and I tried to evaporate the isopropanol under vacuum but instead I got distillation of the IPA and when I poured it to HCl solution it didn't look like oil- it dissolved in the HCl solution (like you can see in the picture).
And i am not sure- I think I still had probably a lot of IPA in the solution and that's the reason it dissolved.
So i have 2 questions-
1. is there another way to evaporate the IPA?
2. is there something I can do to save what I have?

 

[UWe9o12jkied91d]

Normally you can vaccum distill or rotovap the ipa off, maybe your pump is too weak or glass too large for it to come over properly.Anyways, you should precipitate dropwise with energetic stirring and watch closely when it starts to precipitate very little with each drop, check ph then.Additionally using aq. HCl is gonna stump your yields and make side products and color your reaction mass.If you have HCl you just go buy some bleach and a dessicant and do it like gentlemen,

 

[Fenster]

Why would it be any different?

The reduction of MDP2P should run the same as P2P only the purification steps will vary however your amagam process should run the same. I suggest you investigate Jesse Pinkmans work ups he posted from rodium and look into Ritter's work on MDP2P reductions.