The distillate I collect from my EtONO wacker is really fucked up. Instead of one peak corresponding to ketone, I got two. One was around 120C and the other around 150C. Neither was safrole. My vacuum was constant the whole time as well. I even took drip rate vs. temperature data and plotted a graph. The graph showed that there were two peaks in the collection as well. My theory is that both of these peaks are relatively pure ketone, but one of them (probably the higher one) is an azeotrope that the ketone forms with either its polymer or some unhydrolyzed acetal. I suspect this, because I have found that the acetal forms a minimum azeotrope with safrole, even in very small quantities. The lower fraction was pale flourescent green (like lemon-lime powerade) and the higher fraction was more like piss yellow. Both fractions were about equal in size. I have yet to aminate it, as I am trying out a new procedure for then amination and need to perfect it first. I would post the graph I made, but I don't know how. A while ago, I read about someone getting a strange liquid when distilling ketone from a performic rxn, but I can't find the post. Does anyone have any clue whats going on?
