one word.... PARAGRAPHS
Ok, so you extracted the post amalgum mix (disgusting shit) with toly... then you did a brine wash and water wash, good.
Did you sep off the aqueous layer?
You A/B the toly, and...
Once the PH was at 12 he stopped basifying the aqueous layer was a milky white with very light brown oil at the bottom of the sep funnel
the toly would sit at the top of the water.... you had three layers? this has gotten me confused.... or am i reading it wrong?
Your A/B'd toly should be on the top of the aqueous layer, then the milky aqueous layer, THEN you had a light brown oil at the bottom of the aqueous layer???
So you DCM extracted the light brown oil.... do a few more and pool the extracts, make sure you agitate the mix and then leave for a few mins for the layers to adequatly seperate before you sep off....
I wouldnt do another A/B you seem to have done enough, and yes there may be more ketone left unreacted in the toly post amalgum so distill it and find out, more than likely its only a tiny amount (trace) thats giving the smell....
There may well be fb in toly still, but the FB is more soluble in DCM than toly (right??) so if there is it will only be a small amount, sep off the aqueous layer and DCM extract the toly a few times, pool the extracts with your others and distill off the DCM, then setup for vacuum distill and distill the freebase... then gas.
Should be right after that....
-AC