mnick12 - 6-4-2011 at 18:46
Hello everyone,
I have an annoying problem that I hope you all may be able to help me with. I am interested in preparing m-nitroacetophenone for another
experiment. I looked around and found a procedure on orgsyn. Now I have conducted this synthesis 3 times now at 1/10th the scale, and every single
time I end up with same black goop. At first I figured my ice bath was not cold enough. So I ended up freezing one of my flasks in salt water bath
over night. The block was absolutely freezing it took several hours for it to completely melt. But yet again I ended up with same redish black goop,
and it was only through a very tedious work up that I was able to get <2gr of impure product. So what is my problem? I doubt its cooling, and all
of my chemicals are quite pure. The acetophenone is ACS, HNO3 is standard lab stuff, and the H2SO4 is drain cleaner. I was thinking using fuming HNO3
might work better, but I dont really want to do any distillations. However if that is indeed the problem I am willing to do what is required in order
that dont end up with stinky black goop.
Thanks!
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ScienceSquirrel - 7-4-2011 at 02:49
I would say that you are not stirring it well enough so you are getting localised heating.
The mixture must be kept homogenous and cold throughout the reaction according to the procedure.