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Author Topic: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines  (Read 599 times)

poisoninthestain

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #40 on: April 10, 2009, 03:16:16 AM »
Iron is also proven to work on beta-nitrostyrenes.

I've seen ancient references gallore that it's patent proof but nothing recent.

Also, tin should work too but I'm not 100% sure on that one.

If some zinc decides to fall into my lap I pinky-promise I'll post a writeup with pics for a Zn/HCl reduction on nitroalkenes withint the next week.

I'm flat broke so if anyone has some OTC source of zinc I'd be indebted. I've read of successful writeups involving chopped/grinded up pennies as the zinc source. My only question is how the fuck do you cut up a penny?

Vesp

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #41 on: April 10, 2009, 06:49:50 PM »
From my experience you only need to scratch a small bit of the copper coating off of the penny so that the acid can react with the zinc. Once that happens, the acid will eat the penny out and leave a nice copper shell. You probably wouldn't have to cut it up to much, but if you have some nice metal cutters of some sort it isn't difficult to cut them up into several pieces, but it might be a bit time consuming.
Try tossing a scratched penny in some hydrochloric acid, might give you an idea if you can use that.

Alternatively you can melt pennies easily on the stove, take off the floating copper oxide/copper layer with a fork or something and then pour molten zinc into a bucket of water. If you get the zinc hot enough, mossy zinc will be produced.
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Vesp

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #42 on: April 14, 2009, 01:56:00 AM »
Back to the discussion on CuSO4, NaCl, and Al. Someone at The Shroomery pointed out that the amines that are produced from this reduction should form a complex with the copper ions shouldn't they? If there are any copper ions left, that is, which I assume their must be otherwise the reaction would stop, right?

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Sedit

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #43 on: April 14, 2009, 02:41:49 AM »
I think they will.That could be one of the reasons that Klute didnt smell the MeNH3 until the addition of sodium hydroxide. He figured that the amine was locked away in a salt form but it is possible that it is locked away in a copper complex that must be broken. I have just enough Copper sulfate for one very small test run. The rest turned into a blue stain ground into my carpet. Streight from the can MeNO2 is mostly methanol and more then likely dry so im going to attempt it in a small vial directly in the nitro mix. The reaction never does much until the addition of H2O so Ill let yall know what happens. LOL i think Im gonna start my self a random experiment threed just to quarentin all my mad scientist little test I do but dont do right. ;D
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Vesp

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #44 on: April 14, 2009, 03:14:44 AM »
I have been thinking of starting a random experiment thread myself, so go for it! That would be great, I have also been considering a failed experiment thread, I'd be the most to post in that one most likely.

It might be hard to get MeNH2 out since it would either complex with the copper ions, or be in a salt form. This could explain why the smell isn't very strong when it is present. maybe?


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Sedit

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #45 on: April 14, 2009, 03:59:56 AM »
LMAO I think my random experiment threed will be my failed experiment threed. ;D
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poisoninthestain

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Re: Mercuric/aluminum amalgam reduction of substituted Beta-nitrostyrenes to amines
« Reply #46 on: July 16, 2009, 06:43:43 PM »
I should also mention the solvation of DMNS isn't really necessary if you incubate on a plate/stirrer, so you can eliminate the IPA part and just dump:

DMNS + H2O + R'OH + HgCl2 + Al(foil) + GAA + heat =nitro-styrene/propene

Just be sure to add the mercuric salt last. Makes it easier. I use a syringe filled with a liquid suspension of the chloride.

Yields are roughly the same.
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