Hexavalent
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Phase Separations
I have nearly finished a synthesis of hydrazine sulfate via the hoffman rearrangement on urea, but, the butanone azine which is formed just will not
separate out from the other stuff in the mixture as an organic phase.
At the moment, I just have a faint-yellow turbid mixture . . .anyone have any ideas on how to promote phase separation? I was thinking adding
saturated NaCl or even solid NaCl, but I wanted to check before doing it lest I ruin my product.
I am also aware that extraction using toluene and then absorption into the H2SO4 used for hydrolysis also seems to work, but, I have no toluene
available.
Help?
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
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Hexavalent
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I should also point out that I followed the procedure that UnintentionalChaos gives on his YouTube channel, but I used an equivalent amount of
household bleach instead of the 12.5% NaOCl that he actually specifies.
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
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UnintentionalChaos
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Quote: Originally posted by Hexavalent  | | I should also point out that I followed the procedure that UnintentionalChaos gives on his YouTube channel, but I used an equivalent amount of
household bleach instead of the 12.5% NaOCl that he actually specifies. |
What concentration is the bleach? And do you mean equivalent moles or volume...hopefully the former. I would try saturating the solution with NaCl and
see where that gets you. The solution already has plenty of NaCl in it...more isn't going to hurt.
Also, please start using the edit feature instead of multiposting.
Also, also, U2Uing me here and sending me a private message on youtube AND posting a comment to my youtube profile with the same question will not
make me respond faster.
[Edited on 2-15-12 by UnintentionalChaos]
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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Hexavalent
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Posts: 1564
Registered: 29-12-2011
Location: Wales, UK
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Mood: Pericyclic
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The bleach says 'less than 5% chlorinated bleaching agent' or something similar. . . .which makes things quite ambiguous. I actually went 'he used
just over 12%, so, if I assumed that my bleach was 4%, I need x3 times the volume. Stupid, I know.
Can anyone offer any better suggestions?
"Success is going from failure to failure without loss of enthusiasm." Winston Churchill
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