Raf ran peracid oxidation with 300 grams of isosafrole,ended with nice viscous orange ketone,hydrolysed 2 hours at 80-85,washed with 5% NaOH solution and then with water and then distilled.There was little forerun of about 50 grams of so,mainly water and then ketone started coming over,when about 100 grams of ketone had already come over,distillation flask started smoking pretty hard and distillation stopped.Raf was very pissed off.What could have caused something like that?Raf was pulling ketone at 145-155C or so.Maybe he needs better pump.Or maybe he should have washed post hydrolysis mix with Na2CO3 not with NaOH.Has anybody else experienced something like that?
