Do you consider an inert such as an N2 atmosphere an "exotic reagent?"- There are countless papers on this matter-- however, if it appeared that you made some effort at UTSFE, conducted a modicum of research on the topic, and then asked a more clarified and specific question, that even in spite of all that is out there some folks around here might attempt to answer your questions-- maybe...)

  IMO-- the pyridine demethylation, as is, never gives very good yields unless more "exotic catalysts" are utilized, regardless of what sort of rxn vessel is used. It is a dirty, tarry rxn with several by-products that after an acid-base extraction would still require several recrystallizations to render it anywhere near a pure, white crystalline powder. And yes, various chromatographic procedures will work, but most would involve a level of lab technique and comprehension that seem to be a bit beyond what you are presently seeking. And sublimation only really works under certain circumstances, and I am pretty sure that M freebase will decompose after being subjected to total melting, vapourization and then hoping for yr compound to form neat little needles/platlets/helices condensating purely upon the cooled glass sublimation tube surface. I think Casy/Beckett or Bentley mention something about some of this, but it might be more likely to be found in the old late 19th Century British and German papers.

  Best of luck, study thoroughly, UTSFE, and compose your questions to all the folks around here as specifically and coherently as possible-- that's the best advice I can offer...

  Take care

    --Sol

hey enkephalin you wont find too many members with pyridine in their cupboard 

This nest has tried to keep itself OTC oriented ... the 'high tek' semi/pro  lab synths seem to be more for somewhere like SM

Having used the fucking search engine there are acres of opinion and what-ifs regarding demethylation etc, but a real paucity of reports of people actually having done something successfully.

Er their have been numerous successes demethylating codiene to 'other' things ... the SE brings up tons!

I guess you are asking if any members here have had success doing so, AND how they did it! ... have a read around the forum!

 if you can get your hands on some pyridine you're already 3 steps ahead of most of the members here...well at least those outside of E Eurpoe or Asia

 

  I read your OP several times.

  In fact in one of my first posts here I discussed exactly what solvents, in my dreams, worked best for the purification of M from a post-rxn sol'n such as what you are describing. Jon elaborated a bit as well. Look into all those folks trying to extract from plant sources- the process of removing the alkaloids from a dirty mother liquor, then removing any unwanted lesser alkaloids, and then finally purifying the M (hint: usually by rextallization). Not that much different than isolating/purifying from a post-rxn mother liquor, esp. in terms of strategy.

 I apologize for my uncertainly as to the definitive answer to the sublimation question-- but I have never ever once, in several years of researching the topic, come across any report (neither lay/anecdotal nor professional) which describes anything like a successful purification via sublimation for the alkaloid in question. Furthermore, I believe it is discussed in 'The Morphine Alkaloids' by KW Bentley that M would more often than not rapidly degrade upon reaching its MP and even slighly exceeding it. However since I do not have access to my copy of either text ATM I cannot verify and thus must be (gulp) only 'pretty sure' that it will not work as a purification method.
   
  I highly recommend both aforementioned books-- they are both goldmines of opioid chemistry info. And with regard to 'personal experience'-- I believe the first post I made at this forum was about how I envisioned hypothetically a very successful potential purification of M. Jon even elaborated on the topic and talked a bit about why certain solvents/acids/bases were preferable over others (info I largely gained via countless adventures with trial-and-error). So with regard to 'personal experience' I know, with absolute certainly, that there is info of this sort within this forum.

 Damn, maybe that exchange resin shit kicks ass but I don't know how it would apply to a post pyridine demethylation (?)

 Fuck-- if you or anyone else could dream up some kind of successful M sublimation, even if merely as a substitute for a final re-xtal'n purification-- that'd be fuckin awesome! In otherwords, while my own experience makes me doubtful with regard to the sublimation question, by absolutely no means do I discourage you from researching and (especially) experimenting!

  Good luck. Hope that clarified my first post a bit...

      --Sol

you know i wonder if ALC3/pyridine or similar could be used instead of BBr3?
they are both strong lewis acids so they would do the same thing