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Author Topic: phenylnitroprophene reduction  (Read 258 times)

mildronate

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phenylnitroprophene reduction
« on: May 26, 2012, 02:49:56 PM »
Your coments about reducing in large scale? Best method urishibara or amalgam?


This is a prime example of how NOT to start a new thread! You managed to even misspell words yet you only wrote two fucking sentences.
Try to add some valuable data or something when starting a new thread, we have a short question thread for BS like this.

~Sedit
« Last Edit: November 02, 2012, 04:39:33 PM by Sedit »

Electro´S

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Re: phenylnitroprophene reduction
« Reply #1 on: May 26, 2012, 03:19:23 PM »
I have never tried urushibara, But amalgam is something like crazy reaction in one mole scale ::).
If you want reduce more than one mole, amalgam is not the safe way (i think). The huge amounts of hydrogen liberated and the extreme hot would make jump all for the air in any mistake.
Run it allways outdoor is the best advice I can give you and don't try to condense the vapour with standard glassware. Yields are not the best but is not bad. Benzaldehyde is cheap, condensation to P2NP is easy and high yield and with easy OTC reagents amalgam run perfectly.
Maybe P2NP to P2P and them reduction with formamide would be more Large scale than this reaction. Is something i got in mind. Some day i will dream something like this.

carl_nnabis

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Re: phenylnitroprophene reduction
« Reply #2 on: May 26, 2012, 05:05:54 PM »
Uhm... for first i would suggest you dont do larger batches than 25g in an 5000ml flask using an amalgam because nitroalkenes reduce much more exothermic than does a ketimine. The second thing i would step away from the idea using Al/Hg at all, a CTH using palladium on carbon or an electrolytic reduction is the way to scale up here. Theres some information for both out there, look it up at rhodiums archive maybe.
Edit:
hxxp://www.erowid.org/archive/rhodium/chemistry/nitropropene.cth.txt
hxxp://www.erowid.org/archive/rhodium/chemistry/amphetamine.phosphate.html
Those are the methods I was reffering to
« Last Edit: May 26, 2012, 06:57:50 PM by carl_nnabis »
"It's like the drug trip I saw when I was on that drug trip!"

onoone

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Re: phenylnitroprophene reduction
« Reply #3 on: October 28, 2012, 02:46:09 AM »
Hi there carl_nnabis i have been researching for some time now  on reduction on p2np and to avoid Hg, i came across  this reference paper (1) and the post by dreamer on reduction of p2np to amphetamine via pd/c, but i have found out it is not as stated because nitro-alkene is reduced to oxime  ( 1;2;3 )

So my question is why does he state that and he clearly says "amphetamine salt" !!


(1) hxxp://www.erowid.org/archive/rhodium/chemistry/nitropropene.cth.txt
(2) hxxp://www.erowid.org/archive/rhodium/chemistry/nitroalkene2oxime.cth.html
(3) hxxp://www.erowid.org/archive/rhodium/chemistry/cth.af.review.html

ppanik

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Re: phenylnitroprophene reduction
« Reply #4 on: October 28, 2012, 03:36:23 AM »
we do 45g P2NP reduction with al/hg in a 3000ml flask. More will not work in this setup.

Electro´S

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Re: phenylnitroprophene reduction
« Reply #5 on: November 01, 2012, 06:23:20 AM »
Quote from: ppanik on October 28, 2012, 03:36:23 AM
we do 45g P2NP reduction with al/hg in a 3000ml flask. More will not work in this setup.

And Yields was...???

Zinc reduction of Nitroalkanes is not the Panacea in this route (Nitroalkene to aminoalkane) but whith carefull it kicks in the ass Amalgams.

ppanik

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Re: phenylnitroprophene reduction
« Reply #6 on: November 01, 2012, 10:52:48 AM »
expect it, from the 45g P2NP we get about +35g Amphetamin Sulfat (nice white)

(at starting, every thing comes from the refrigerator!)

mildronate

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Re: phenylnitroprophene reduction
« Reply #7 on: November 02, 2012, 10:58:39 AM »
Palladium is imposible. How about reactor cooled with dry ice + ethylene glycol?

onoone

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Re: phenylnitroprophene reduction
« Reply #8 on: November 02, 2012, 12:04:03 PM »
I was wondering how important is acetic acid in reductive animation with al/hg, and can i substitute with some other otc solvent like ethanol ? thanks

lugh

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Re: phenylnitroprophene reduction
« Reply #9 on: November 02, 2012, 04:44:13 PM »
Quote
I was wondering how important is acetic acid in reductive animation with al/hg, and can i substitute with some other otc solvent like ethanol ? thanks

It seems we have yet another ignorant newbee attempting to take shortcuts  ::)  The subject of this thread is nitroalkene reduction, not reductive amination  ???  Members of the Hive researched the old chemical literature and someone called Sunlight attempted the reduction with acetic acid and reported success  :P  Members of Hyperlab improved the procedure's yield, which is documented on Rhodium's page  :-X All of you newbees need to study these matters long enough to understand what's going instead of asking someone to tell you   ;)  There's no need for a new thread with more stupid questions on this topic so often  >:( The end results from the effort applied  8)
Chemistry is our Covalent Bond
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