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 731 times
Klute - 1-9-2009 at 08:26
Did the solution heat up to 60-65°C? Maybe you should activate your zinc before use..kmno4 - 1-9-2009 at 08:45
Did the solution heat up to 60-65°C? Maybe you should activate your zinc before use..
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.
