Osmium, in trying to purify asarone ketone, I found that:
1) it was destroyed by distilling at atmospheric pressure (unlike mdp2p, pmp2p)
2) using the oxime formation as a purification step gives nothing other than a sludge (that aminated!)
3) bisulfite purification doesn't work, as it gives the typical impure chicken fat result that MaDMAx is showing off in the pictures above
Can you please clarify what you mean by add a bit of NP and shake? Are you saying that beautiful bisulfite crystals of tmp2p will form if I add some NP (what would you recommend, DCM, toluene?), aqueous bisulfite, and stir? I notice in other posts you recommend not to use alcohol, did you use it when using a NP?
Thanks.
PS. MaDMAx, I was going to take pictures exactly like yours! Really! I was! I'm just lazy. =) I was going to do it in 3 or 4 test tubes though...