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Al/Hg Nitro Synth regarding flask size ???
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IndoleAmine
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: Al/Hg Nitro Synth regarding flask size ???

 Tue May 10, 2005 7:04 am		 Reply with quote
Your SWIM doesn't do reductive aminations with a ketone and methylamine - he does nitropropene reductions AFAIK... Wink

(red.aminations which generate methylamine in-situ from nitromethane are far more exothermic!!)

And 20g P2NP in a 3L is no problem - try 12g P2NP in a 1L with slightly crumbled foil (no nuggets) and 200mg HgCl2 at once and you'll run into trouble (well almost, unless you happen to have a superb double-surface 300mm condenser.. Twisted Evil ) - btw this condenser was taken to 1/3rd reflux height for the first time ever during the mentioned reduction using a 1L flask - it was f*****g scary (and very hot, absolutely not touchable) I was told, with alcohol fumes coming out of the condenser and immense fizzing and a decent "pshhhh" sound all the time... Shocked

Thats why thick Al is better sometimes. For example.
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Bumblebee

Joined: 26 Mar 2005
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re: Al/Hg Nitro Synth regarding flask size ???

 Thu May 19, 2005 4:45 pm		 Reply with quote
Quote:
try 12g P2NP in a 1L with slightly crumbled foil (no nuggets) and 200mg HgCl2 at once and you'll run into trouble (well almost, unless you happen to have a superb double-surface 300mm condenser.. Twisted Evil )


IndoleAmine: Do you have installed a spy-camera in my kitchen? you didnīt look at it rightly, there was 12,2g P2NP, and the foil was totally uncrumbled... I did use a 400mm Condenser, and everything did look much like in cape canaveral when a space shuttle is taking off. just with the difference, that this rocket seemed to try to fly downwards Wink

Really: there was such a steam pushing out of the flask, that i had to wear a gas mask immediatly.

So did i watch through my yellow draeger-mask the reaction goinī to completition while swirling it in an ice bath...

The rxn did stop 1 or 2 minutes after the P2NP in AcOH was added. Really a Turboreduction, in a total time of 10 minutes after beginning the amalgamation with hot (dumb!) water...

i didnīt expect anymore than 1 or 2g of product, but there were at least 6g of very clear white amine, after extracting, wich i fucked up later while crystallizing... (as usual Wink
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