Into the standard 2 liter pop-bottle/tubeless tire valve pressure chamber:
1 g PdCl2
5 g CuCl2 (anhydrous if it matters)
150 ml MeOH
1 ml dH2O
Prestirred/dissolved, then:
50 ml safrole
A word of warning, solution must be acidic for the wacker to run, so test the pH and adjust as needed.
Plugged and sealed, pressurized to 40 psi with pure O2 from a tank (regulator hose hacked to accept a tire fill adaptor). Vigerously shaken by hand for a few minutes for good measure, then left on it's side to maximize the O2/solution surface area. Come back and shake the hell out of it on a few occassions say once every half hour for a few hours, details dont seem to be important. At about the 4-5 hour point the bottle was purged, repressurized with more O2, and left at room temp on it's side for a total of about 20-24 hours. The sides of the bottle should be noticeably 'soft', much less hard than when first pressured. In the past when I screwed this up it was due to lack of proper pH or lack of patience, this batch size will draw about 25-30 psi down total.
Workup:
Dump the reaction mix and about 100 ml of 10% HCl into a sep funnel. Realy don't need to shake, the ketone/oil will precipitate out by itself. After draining off (and keeping) the bottom organic layer, extract the remaining aqueous layer a time or three with a non-polar. Toluene or xylene work better at getting all the tar and shit out of the aqueaous layer IMO, which is important for later. Keep both layers.
So, you have the toluene/ketone/crap fraction in one container, and the water/acid/alcohol/catalyst in another. Wash the organic layer with distilled water and add that water to the other aqueous stuff. This should leave you with most/all of the catalyst in the water/alcohol.
Vac distill the organic layer to get the ketone, a water aspirator is good enough. On my rig the light yellow spicy smelling ketone comes over at about 145C. Yield: Consistently 38g MDP2P from 50 ml safrole, almost certainly higher if you have a better vac source/still. If the reaction was allowed to run to completion there shouldn't be more than a few drops of saf/isosaf. Likewise, no real sign of the aldehyde...except for some polymerized crap the reaction seems to run very clean. OK, got the goods...now to the catalyst.
If you properly extracted the aqueous layer there isn't going to be much in there besides the metal salts, HCl, water, alcohol. Distill/boil off the volatiles to leave a residue of our happy catalyst, ready to be reused. So far I'm up to three re-uses with no signs of quitting, should be almost indeffinately reuseable (after all, where can it escape to?) Just make sure you extracted that aqueous layer well or you'll get a tarry mess when you boil off the water/MeOH.
And there you have it. Shit easy, pretty much full catalyst recovery, decent yields...and if you pay attention to pH and use O2 it seems to be very very very reliable and reproducible. For what it's worth, it seems to work equally well increasing the saf to about 75 ml. Al/Hg amination, the honey is sweet (I get about 14 g honey.HCL for 20g ketone, some bad procedure I think.) Happy cooking.
Oh yah, where to get an oxygen tank? Just go to a bulk gas place, the sort that sells gasses for welding and blow-torching. Tell em you need it for your propane blowtorch if they ask, O2 is completely unwatched so no worries. Usually rent the tanks on a yearly basis plus fill/refill costs. Figure $60 for a year and a fill. Another $150 maybe for a regulator, you can figure out hacking the hose.
Legion Bob
"We're Everywhere!"
