Acidic Hg/Al amalgam

[sYnThOmAtIc]

Man what the fuckk?
"In case your not familiar, there is no MeOH used and amalgam is done with water prior to dripping in MeNH2 and ketone (both in IPA solution).  As a matter of fact, they're not dripped in at all, they are simply added." 
HENCE THE REASON YOU HAVE SHIT ASS YIELDS.

You obviously have not done this procedure correctly. Nitro redcutions and brightstars meam though good but seriously outdated yielding only a mere few grams form 50g ketone HAH, Are not carried out the same.

You mention the preparation of amalgum  ad the water and al/hg for storage purposes in certain liquids if you'd rather have pure al laying around instead of hgcl2, and meoh is present with NO (or very little~5%)water when you do this readction with the amalgamation preceding it in the same container with no washings. Meoh, hgcl2, al simple it bubbles gets dull and foggy and boom you ad your shit. Yea go ahead and dump 50ml of nitro and 75g of ketone into the flask at once and you will bath in it. I would rafrain from saying what I don't know what I'm doing when who I've tought is getting high eighty to low ninety percent yields.

You wonder why you don't get the fruits of your labor? Then wake up and figure out how to do it correctly!

https://www.thevespiary.org/rhodium/Rhodium/clandestine/gonzo/index.html

Follow this and you may have better luck.

[Moriarty]

I think your under the impression that I was accusing you of not knowing your shit.  Never meant to imply that.  I've read my post a couple of times and still don't know how you came up with that idea.  You mentioned not getting a volcanic reaction.  I too got no such reaction.  However, you didn't really specify which method you were using, so I simply told you which one I was using.  I know the difference between the methods in the BS write-up and those set forth in the MM write-up.  That wasn't my point.  I was merely concurring, to a point.

To the point.  Unless I read it wrong, I did the amalgamation correctly.  In the BS write-up I had (possibly out-dated) you start with water and do wash before MeNH2/Ketone in IPA are added.  Pretty sure the copy I had stated just that (I've read it a hundred times).  I now realize, through trial, error and advise recieved on the Hive, that it's supposed to go down like you said.  Thanks for the advice, I really do appreciate it, I don't take myself too seriously and never meant to imply you don't know what your talking about.

By the way.  Didn't this discussion start out on the topic of Acidic Amalgamations?  There are certain problems presented if your doing this with MeNH2.HCl and having the mixture acidic, but my textbook understanding of the process would tend to point me in the direction of an acidic solution.

[goiterjoe]

moriarty, if you can just dump in your ketone, then it isn't ketone. 

I've also used HgCl2 still in the water it was made from to fuel an Al/Hg reaction, and it ran quite smoothly.  I didn't think it had anything to do with the acidity though, I think it had more to do with the few drops of excess H2O helping to cool the reaction and to provide water for the formation of aluminum hydroxide and free hydrogen to reduce the imine to the amine.  Without these few drops of excess water, all of the water required in the reaction will have to come from the ketone to imine formation. 

OK, I guess that didn't make much sense after being written down.  But I know what you're talking about.

If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music

[Moriarty]

I think there is a difference between the process when MeNH2 is used as opposed to MeNO2.  That's what synthomatic was saying and that is what is indicated by comparing the MM write-up to Brightstar's.  What you wrote did make sense and I agree, it doesn't go very fast when the only H2O in the picture is that produced by imine production.  Thanks.

[sYnThOmAtIc]

"In case your not familiar, there is no MeOH used and amalgam is done with water prior to dripping in MeNH2 and ketone (both in IPA solution).  As a matter of fact, they're not dripped in at all, they are simply added."

As for all amalgamations I have noticed on pinkys results that any reaction where the hgcl2 was dissolved in water or meoh and the al allowed to react prior to reaction and replaced with fresh solvent with ketone later added, a substantial loss in yield was incurred (even in the calssic BS).  Even with meam there are better higher yielding ways than the bs writeup. He gave a working method for the non-chemist for fun based product not high yielding street slinging tweaked procedure.

[Flip]

I don't even claim to be highly knowledgeable on that subject but I think that the lower yeilds would have more to do with the timing of the amalgamation and the timing of the drip..... I don't see why the acidic solution would hinder the reaction and i'd imagine that having it in this medium would allow for better dispersal of HgCl2 around the Al for amalgamation.  I dunno that just seems logical.

Flip

[Chromic]

Acidic conditions ruin yields.

This is my theory: the methylamine forms the more stable methylammonium salt and will no longer act as a good nucleophile and will not attack the carbocation of the ketone (protonation of the carbonyl, one would think would improve reactivity... but it doesn't seen to, the more important, reaction limiting step is making the methylamine a good nucleophile and not making the carbonyl a good electrophile). Bright Star's yields suck because he does not add enough BASE to his reaction to turn the MeAm.HCl into MeAm. The general idea of Bright Star's method is, in my humble opinion, superiour to Methyl Man's. I've tried them both, and prefer (and gotten better yields from) BS (... but done in MeOH with 1 equiv base and a toluene extraction).

Both methods work, and what I think should decide if one uses MM is if the reaction size is small and it's a relative pain for you to produce methylamine. (but if your reaction is big or it's easy for you to produce methylamine, try Os' approach... you won't be disappointed)

[Vibrating_Lights]

ANTIBODY.  DOES THER AL HAVE TO BE PREPARED SEVERAL TIMES WITH WITH A RXN LIKE THAT OR CAN IT BE DONE ALL AT ONCE AND THE AL JUST SCOOPED OUT OF THE POT AS NEEDED.  THE hG IS ONLY REMOVING THE OXIDES CORRECT IT IS NOT AFFECTING THE ELEMENTAL AL.
VL_

[Rhodium]

VL: Please check your caps lock status before posting a message. That post was really ugly.