kmno4
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N-phenylhydroxylamine..... ?
I tried to do this:
http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=CV1...
(also in attachment)
There were 4 runs, two with 10g of nitrobenzene and two with 5g.
All attempts gave ZERO percent of phenylhydroxylamine. I used different amounts of Zn powder but results were the same: lots of white powder (ZnO) and
milky solution. After adding NaCl and cooling, some droplets (in small amount, blackening in the air) started to separate. Droplets were dark-yellow
and not solidify even at -10 C.
What am I doing wrongly ?
Maybe someone has any good results in preparing this substance by this method ?
[Edited on 1-9-2009 by kmno4]
Attachment: cv1p0445.pdf (158kB)
This file has been downloaded 810 times
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Klute
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Did the solution heat up to 60-65°C? Maybe you should activate your zinc before use..
\"You can battle with a demon, you can embrace a demon; what the hell can you do with a fucking spiritual computer?\"
-Alice Parr
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kmno4
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Yes, mixure becomes almost hot at some stage.
My zinc reacts completly to ZnO.
In Gattermann there is similar synthese but with keeping temp. ~16 C and yield is "almost quantitative". In another paper it is written that "almost
quantitative" is bullshit and Gattermann is wrong.
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