the ketone was a lemonade bright neon yellow color
during the reflux was flowing down to the reaction flask  continuously
there was no safrole prerun after the dcm came over there was no safrole that came over in the recieving flask.(Im so stupid to not remember that)
nitro came over at 101cel with no vac
electronic scale measured the hg and 200mg was added i didnt have the 2l flask yet so i was working in half batches from what methyl man recommended

Are you being a bit aggressive in your distillation, per chance? Write up how long the process is taking you, please.

Your description of ketone sounds reasonable, although it's hard to say for sure without seeing and smelling it.

-ketone

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.

I noticed that there was only a faint Methylamine smell during workup. Turns out what I thought was pure Nitromethane - I distilled in from fuel like you - was only 50% pure. What % Nitro was the fuel you used? Did you dump everything prior to hitting 101 C.?
SWIM went and bought 99.99% Nitro instead and next time workup smelled like girls lockeroom tampon can...
Do yourself a big favor and buy a Vacuum pump! You can get a belt drive pump for $100 on auction and it will pull 1 micron vacuum all day long! SWIM gets his Ketone to come over at 105 C.

Another good thing for first timers is to make the darn MeAm rather than trying to do it in situ. It's not hard to make, and you can make it fairly damn pure....and the reagents aren't hard to get at all, even for lab grade.

I wouldn't trust ANYTHING I get from a hobby supply store For all you know, R/C car fuels might have all sorts of minimal added agents that could help inhibit the reaction, or cause side products.

-ketone

Think bigger than RC you might bee OK!

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You can tell the queen of diamonds,by the way that she shines.-GD

i finally went out and got everything i needed. i got myself the much needed vacuum pump. im attempting to distill for the ketone as we speak. however, im having a problem. first of all the dcm came over around 60c. the safrole is coming over at 120 degrees. but for some reason it seems that while the safrole is coming over, something is crystalyzing in the vig column. i have the vig insulated with glass wool, i dont have any leaks, and im doing this under vacuum. the crystals seem to be the color of the safrole. i dont know if im doing anything wrong. im going to continue, if ive fucked up at least i will know where i messed up at. the saf. is still coming over. got to play the waiting game for now.

DCM should come over at 40C at normal pressures (1 ATM) and under vacuum it should come over at less then room temps.

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Sink or SWIM

i think the crystalation was caused by the lack of sufficient insulation. i will redo everything.

safrole doesnt crystalize when you distill it...PERIOD

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Sink or SWIM

do yo have any idea what it might be?

Ive never seen anything crystalize when heating it up e.g. distillin it. Because when you heat a substance it shouldnt crystalize. There are only a few compounds that have lower solubility in higher temps.

Its probably some kind of polymerized thing. most likely bunk sassy...

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Sink or SWIM

quinone?

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Loriel... because Im worth it!

well, im doing it over again. the dcm is coming over at about 42 degrees. well see.

well, i started doing Reductive Amination of MDP2P with Al/Hg + Nitromethane by Methyl Man. im using the recomended aluminum, the right amount of meth and everything else. last time i did this i had no problem with the aluminum dissolving. however this time, i must have done something wrong. the aluminum is not even bubbling up. the only differnce between this time and last time is the methenol. last time i distilled it from rc fuel while i was distilling nitromethane. this time i used methenol i bought from a company. also the hg that im using is not disolving completely. if that makes a diffierence i added more methenol as recomended by rhodium. however it is not dissolving completely. im using HgNH2Cl, i dont know if that makes a difference. maybe i need to crack a thermometer. if thats is the problem.