Anyone here done the Baeyer-Villiger to p2p?

[Rabidreject]

Hi,
I have been messing around with an aldol condensation type reaction on benzaldehyde with MEK in acidic conditions, then a Baeyer-Villiger reaction on that with H2O2 to obtain a p2p ester followed by hydrolosis.
Has anyone here done this? It’s just not a reaction I see mentioned much around here and I sort of wonder why because it worked really well for me.
I would much rather just go from the aldehyde to the ketone rather than having to use valuable nitroethane to go via the nitropropene…also benzaldehyde is plentiful and cheap…
I had much better yields with this than with the nitroalkene reduction (granted I probably chose the worst yielding gross method but still).
How are most people making their p2p?
Thanks

 

[loadingST]

Yes its very easy method i do it very ofthen, just gassing with cooling, isolating the precipitate, then the peracid oxidation and then naoh and its amateurish and otc, my most preffered method to obtain my bmk.

 

[methyl_man_2025]

do you have the detailed method using H2O2?

 

[Rabidreject]

Yeah I’ll write it up for you later.

Performed it first on a smaller scale just to see if I could get it to work, but looking at my TLC it looks like the first step didn’t go to completion or my eluant system was a bit messed up.
So the oxidation step didn’t go as light as I expected and blah blah blah. Final yields were bad but I KNOW it can be done better than that.
So I did another aldol condensation last night and also got some 30% h2o2 delivered this week - last time I took a 12% solution (as it was the strongest I could buy) and I put it in the freezer until some water started crashing out as ice and then I used that. I think it concentrated it a little but yeh I want to try it with 30%.

I’m just working my way through it and will write it up when I complete it.

I swear every p2p synth I have done so far is most horribly smelling shit in the world! The actual smell of the ketone is fine for the most part but dam these intermediates

I actually am totally disinterested in the meth-amphetamine but I was wanting to practice this…im wondering if it’s likely to cleave the MD moiety. Not sure