The losses will really be minimal you may have lost a little bit but the bulk (if not all) will still be there, I sincerely do not think you fucked it up! Not a perfect scenario but you are good.

swim can also back up what was said above.  any losses are probably pretty marginal.  proceed with vac distillation.  swim used to use toluene to extract with and distilled it off atmospheric over 100C.  no worries.  just store in freezer when necessary to store it but i don't think it's quite as reactive as it's reputation leads it to be.  distill away

Quote from: NeilPatrickHarris on April 06, 2010, 05:01:31 PM

swim can also back up what was said above.  any losses are probably pretty marginal.  proceed with vac distillation.  swim used to use toluene to extract with and distilled it off atmospheric over 100C.  no worries.  just store in freezer when necessary to store it but i don't think it's quite as reactive as it's reputation leads it to be.  distill away

Can you elaborate on how you were able to distill with toulene?  Is it some sort of azeotropic mixture? The vacuum is quite noisy and if I could avoid using it somehow it would be of great help.

edit: Nevermind, now I see what you were saying.  Simply out of curiosity, is there anyway to separate my ketone without using vacuum distillation?  Seems the bisulfite addition is quite messy and a yield killer when used with an impure reaction solution.

sorry for any confusion, swim saw how you were concerned with having subjected your ketone to 100C for an extended period of time twice.  i was just reassuring you that it is ok.  swim used to extract ketone with toluene.  he would wash the toluene as normal and then distill the toluene off atmospheric at 110+C and then let it cool down, change to a smaller flask and vac distill the remaining crude ketone.  i was just saying swim subjected his ketone to similar temps on a regular basis and never had any problems come from it.

as far as isolating the ketone without vacuum distillation, yes there are ways but you should not pursue them.  definitely stick with vacuum distillation, no question.  swim has experimented with non-distillation purification of ketone via bisulfite complex and steam distillation (co-distilled with water).  the problem you run into with the bisulfite complex is that if your ketone is too crude (which it will be) then you'll have trouble getting it to crystallize.  it's like trying to crystallize mdma from freebase with garbage in it, it won't crystallize properly.  bisulfite is better used as a test, after the ketone's already been purified, at least IMHO.  the steam distillation worked but it takes several hours of distilling and several liters of water, it's really lots of labor.  then you have to extract from the hydrosol and distill off the solvent again, no thank you.  crank up the vacuum and distill it that way for sure, will take a few to several hours but it beats all other methods hands down

To be honest, I haven't used a solvent trap for anything.  I can obtain pump oil at a decent price and have a bit of it, and I just pull the pump apart quarterly or twice a year (depending on use) and clean it out.  The cynmar pumps are tanks hahaha.

well said disposable stirbar.  the only thing to really keep an eye out for is to make sure you do brine washes after the NaOH washes to remove residual NaOH.  base catalyzed polymerization of the ketone is a real threat but will only happen if you're really sloppy.  but all in all, ketone is much more durable than they say.  i'd still treat it like a lady but realistically i wouldn't sweat it too hard if i were swiy.

I just saw the tube collapse bit. Use the heavy walled clear tube with the white cris crossing reinforcement in it. Heat it up in hot water before pressing it on to things. Works great. Never had a collapse.

Sorry for opening old thread but I had unusual problem...

Really powerful aspirator vacuum setup was built and safrole is distilling at 116,5-121°C
and ketone around 160° (my thermometer is marked only to the 150°C)
BTW,thanks on halp and advices,will put sketch and detailed description in new thread
to help others build it when I learn how those part are called in English. 

First time extraction was made with xylene, distillation rune great and more than 50%
VERY pure ketone was obtained rom this first run.
(Allegedly pure ketone is "alien" transparent green and has lovely smell that reminds me on some old bubble gum,
smell is not as intense as safrole. It doesn't freeze but becomes a bit viscous and reminds transparent in the freezer)

Other extraction was done with DCM, unfortunately it was very hard to get rid of all NaOH washes without much loses so I did 3 washes,
resulting in green organic layer.

Distillation was firstly done without vacuum and DCM came in form of emulsion that shown basic reaction with litmus.
Only thing I used that contains nitrogen and smells like ammonia is DMF,so it is that or NaOH somehow 
reacted with DMF resulting in NH4, which explains b.p. along with DCM.

Emulsion of everything was coming at arrund 100°C, evens some ketone and safrole came at cca 110°C.
after some time temp. was stabilized at 131°C and only green liquid was coming out.(it does look and smell like ketone)
After some time temp. dropped (last time nothing more came and it was sign no more ketone was available)
but something organic also came this time close to the safrole temp. (!? (iso)safrole !?)

Even some red oily thing that smells like ketone came, but my guess is that might be polymerized ketone
because of some NaOH present.

I ended up with mixture that has few water drops in it,smells like ketone,but it is slightly more yellow than pure ketone.
When in fridge it becomes emuslion.

My question is how to get pure ketone from that mixture?!

Since ketone is highest boiling fraction in mixture, can I simply dry mixture with MgSO4 and heat it under vacuum
until everything else goes away!?