If the rxn got violent like you say it did, then you either have two problems. Either you did not have ketone, or you fucked up on the workup. Did you perform the workup EXACTLY as methylman details? If not, what did you do differently. You say that their was constant reflux while adding the reactants. Was it a constant stream (no drops). If it was not, how fast was it dripping. How strong was the MeAm smell a/f the rxn? Your ketone couldn't possibly have all come over at 180; what was the range? Determine the pressure of your vacuum using the method I detailed. More than likely, you did not have ketone, and your problem lies with the wacker. How much distillate did you collect while distilling the wacker product? How much safrole did you use in the wacker? Most aspirator pumps, in my opinion, are not powerfull enough to distill ketone. Did the distillate freeze when you stored it in the freezer? If it did, then you maily had safrole. If so, your pump only pulls about 180 torr, and your ketone wouldn't come over until 220C, at which it will rapidly polymerize. How much crap was left in the flask after distillation? I suggest that instead of following MM's workup procedure, you basify it with 300-400g of 25% NaOH. The aluminum should coagulate and crash to the bottom and you can filter it. Then, neutralize the pH and strip off the methanol under vacuum. Take the water/freebase that is left in the distilling flask and bring the pH up to about 12. Extract this 3 times with about 50 mL of toluene. Then perform a typical A/B extraction and strip off whatever solvent you collected the freebase in after the A/B. Distill the freebase (20-30C higher than safrole) under vacuum and gas it. This way, you can weigh the freebase b/f you gas it and know exactly how much you got. Also, try to replace your aspirator with a real vacuum pump - preferably a refridgerator evacuation pump.
