Ketone smokin...

[raffike]

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?

[GenericVersion]

was there a vacuum leak, SWIM notices that sometimes after vacuum is released smoke forms, never seems to hurt product though

[abolt]

Raff, maybe you still had some naoh in there.

BTW, you don't need to use Naoh, just wash twice with saturated Bicarb.

Post 336996

(Rhodium: "Base-catalyzed polymerization of P2P", Chemistry Discourse)

[raffike]

Hmmm...that's possible,will wash with bicarb next time.145-150 C shouldn't bee to high for ketone.