pickler - Seen that doc, read it numerous times, thanks though!
Chromic - Many thanks for the reply. That other oxone thread is getting crowded, so a few more questions if you don't mind.
>If you buffered it as I wrote in my document,
Yeah, 45g of bicarb slowly added, had an initial pH of about 6.8.
>I would recommend that you carefully distill
Do you remember what temps did you were seeing for the epoxide to distill over? I know you mention the 200 degree mark. Did you heat first, then distill? Or did you just slowly crank it up until the ketone started coming across?
>Taste PMMA if you dare
Dare seems an appropriate word here. That's why the comment was made above about not being concerned about yield. The bee in question might not even bother to aminate. Who really needs 10g of PMMA.HCl in their life?
This does bring up a larger question though: Psychokitty mentions trying to acidify the post reaction mix with H2SO4 instead of HCl. This naturally leads one to consider the possibility of a one-pot oxone/rearrangment (using iso-saf of course). After 5 hours of oxone, add sulfuric, reflux, extract with DCM, and distill. Although I guess if thermal rearrangement of iso-saf turns out to be viable it will be a moot point anyway. Just thinking out loud.
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