I'm still just researching it, but I hope to give it a go. Do you think that setup will work? Are you buying or producing the DMA? I wonder how the reaction would go with just air pressurised to approx. 5 atm. I suppose experimentation is king!
check the ref, palladium catalysed oxidation of naturally occouring allybenzenes you got for me,
interestingly it notes that DMF was used under the same co catalyst free conditions and yeilded 84 yeild of the methyl ketone with high selectivity, as in, only 6% of the aldehyde was generated.
the rxn just ran slower, i believe the conditions were, 10atm pure 02, 60c for 6 hours. 1-2% mol PdCl2 catalyst
this is a contrast to another ref that said DMF yeilded nothing. I am inclided to believe that is a mistake or something as i see no reason why it would be so inneficient
I have seen several refs that describe DMF as also being able to keep PdCl2 catalyst from deactivating, just not as effective as DMA
IMO the most attractive thing about the 02 DMA wacker is the abitlity to extract the ketone from the DMA catalyst solution with heptane,
add more alkene and continue the rxn with almost the same yeilds the second time around. I am not sure why this cannot be done with DMF..
From what i can tell, these oxidations ran the same from 5atm - 10atm so 5atm will suffice, but pressurised with only air.. I am not sure. Every singe DMA wacker i have seen was super high yeilds,
none of the refs seem to test the boundrys of just how low you can go with pressure and RXN time. some ran for 3 hours at 60C with 90+ conversion.
I think there is a chance air would work, becasue the reaction is so selective in DMA without copper co catalyst, the ketone is virtually the only thing being made.
If you did it with air, i would take it upto 70 - 80 psi, also, an idea i had was to take apart an electric hot blanket, take the wiring out and wrap it around the vessel, then duct tapethe whole thing..
that should keep it close to 50-60C not to mention the heat generated from auto shaking (jigsaw, or reciprocating saw) it actually gets that hot on its own if it shakes hard enough..
DMF and DMA are both pretty toxic, i wouldnt be playing around trying to make it, if i were you id try to buy it.