Probably best to just give it a shot the way Organikum suggested, as it's already a proven procedure.

The reason to mention the insolubility of MeNH2*HCl in DCM is twofold: one, it means extracting MeNH2 from DCM with aqueous HCl should be trivial, and two, you may be able to gas it out (if your DCM is dry). Alternatively, if the sulfate salt is insoluble (probably is, but can't speak from experience on this one) you may be able to crystallize it by adding sulfuric acid.

fish, what advice have you given that I am ignoring? Yes, I'm aware that the Al/Hg is proven and that this has apparently been done with tin. However, my goal here is to do it with iron as it is cheaper than tin, and less dangerous than working with mercury. Sorry if my reasoning here doesn't jive with you, but I'm the one pursuing this procedure and you're more than welcome to just..not participate.

That aside, I do appreciate your pointing out that the procedure for aromatics won't work for aliphatics. I was not aware of the substantial difference. As I mentioned before, my formal education is a bit lacking.

Did someone found out the patent for nitromethane/ethane that Krause references? I found no patents applied by Krause for the time before 1916.

I tried to locate it but no avail whats not surprising as many patents from this time are listed without any information given, no inventor sometimes not even a headline. Then without number, no chance to find it. It may also be deleted, many patents from this time were deleted just before the winners of WWI could take them for reparations as established in the treaty dictates of Versailles.

A similar problem arises with the patents of the GDR which are hard to impossible to find by normal means and they had a lot of great stuff on ergot for example...

/ORG

Probably best to just give it a shot the way Organikum suggested, as it's already a proven procedure.

The reason to mention the insolubility of MeNH2*HCl in DCM is twofold: one, it means extracting MeNH2 from DCM with aqueous HCl should be trivial, and two, you may be able to gas it out (if your DCM is dry). Alternatively, if the sulfate salt is insoluble (probably is, but can't speak from experience on this one) you may be able to crystallize it by adding sulfuric acid.

Are you referring to Organikum's procedure on sciencemadness?

Any thoughts on your hexamethylenetetramine procedure compared to the nitromethane reduction?

Any thoughts on your hexamethylenetetramine procedure compared to the nitromethane reduction?

The hexamine method I posted times ago is not invented by me but it is the adaption of Hexamine on a patent of the IG Farben using formaldehyde.
The patent was referenced by Org.Syn. thats how I discovered it.

The method is simple but timeconsuming. Very timeconsuming IIRC.

The iron reduction of nitromethane to methylamine is comparable quick and results are good to excellent.

Anybody having access to nitromethane and owning a decent overhead stirrrer is better off  with the iron reduction. In special when scaling up is an option/necessity and time pressing.

It mostly depends on what one has available I would say as best would be to have a big bottle full of Methylamine-gas and thats it.
But if you are in any hurry and free to choose then nitro is the way to go. Hexamine is still better then having to use nitro in methylalcohol as this azeotrope is a pest taking out most of the fun and advantages.

Pick your poison.

@sw0lepapi420: Cast iron filings is what is used traditionally in the Bechamp process and all offsprings, tendency shifting to catalytic/hydrogen reduced iron powder albeit I believe thats more to the benefit of chem suppliers then the reaction (exceptions exist).

But STEEL wool and heavy gauge sheets of what I guess is mild steel, thats rather daring in my eyes and as long I dont see one, better more references from literature or acccounts of somehow respected members of the community I regard this as utter bullshit, low yields if any at all and a parade of byproducts spurned by what makes steel different from iron.
And completely superfluous for iron of good quality and purity can be bought for asscheap by anyone, by the ton in all screenings one might imagine.
So there is no point in the suggestion except mischief or intellectual underachievement count.

regards
/ORG

On the other hand, the galvanized coating of some steel products would have to be dealt with if it was to be used in a reduction.

Just for curiosity: What mesh size would your steel-sheets refer to? Estimated? 

Steel sheet doesn't come in mesh, as far as I know.

Cast iron filings is what is used traditionally in the Bechamp process and all offsprings, tendency shifting to catalytic/hydrogen reduced iron powder albeit I believe thats more to the benefit of chem suppliers then the reaction (exceptions exist).

But STEEL wool and heavy gauge sheets of what I guess is mild steel, thats rather daring in my eyes and as long I dont see one, better more references from literature or acccounts of somehow respected members of the community I regard this as utter bullshit, low yields if any at all and a parade of byproducts spurned by what makes steel different from iron.

You are apparently ignorant of the distinction between iron and steel: carbon steel is higher purity iron than cast iron, which is a crude iron rich in carbon impurities. Almost all commercial iron contains some amount of carbon. 'Steel' is just a term to designate iron with a carbon content that falls within a certain mid-range (typically 0.1% to 2%, with 2% being considered 'ultra-high carbon steel'): cast iron and pig iron contain a high percentage of carbon (>2%), wrought iron contains a low percentage, and steel is intermediate. To make steel, oxygen is blown through molten cast iron to burn off some of the carbon and other impurities.

The fact is you don't need electrolytically refined 99.99% iron to do reductions. Carbon steel dissolves in acid just fine. "Even" cast iron is pure enough.

I surveyed your posts and adore your attitude, the more it is not backed up by anything. Nothing. Nada, Nil. No flesh just pose. Isnt that horrible ardeous? All this pretending and what for? Just to get ridiculed by old idiots like me?
Hereby I pass you a bucket full of pity.
Keep it well, you will need it.


/ORG 

Rest assured, all of my conjectures are educated ones and I have always made it clear which of my posts are opinions and which are based on experiment. Contrasted with the tone of my posts, your posts are a forest of statuesque assertions. As for the topic at hand, I can only assume you have exhausted whatever tiny amount of constructive criticism you had to begin with. With that in mind, sir, it is time for you to "put up or shut up".

I have to add some points to the procedure posted by me here:
http://127.0.0.1/talk/index.php/topic,3571.msg35383.html#msg35383

1. "Good" active iron must be used, if in doubt activate it by defattingwith a suitable solevent and a quick wash in diluted (5%) HCl.

2. In bigger batches the nitromethane must be added in portions over time or the reaction will froth over, whats a unpleasant experience in special if you are not keen cleaning your lab.

The procedure is similar to the one in the attached article which btw. references Krause.

/ORG