Same for the PdCl2. Its probably better to put the palladium directly in the SRV via funnel, than to put it in a separate beaker and trying to do the mixing beforehand. The reason why is that the shit sticks to the beaker and is hard to recover when transferring containers.

When you get it all in there, assemble the unit and THROW IN A STIRBAR before you plug it up with the valve stem...this is a minor improvement that makes a BIG difference, because it enables you to get a much more turbulent agitation of the mixture...and that increases the oxygen uptake dramatically.

This was done next;

Plug the unit. Pressurize it w/ the pump.

I have found that you cannot run the electric tire pumps off of a small battery charger because it doesn't have the amps. Go out to your car and pressurize on the ground beside it. Or take a car battery and set up a work station at a bench, whatever.

Pressurize it for ten seconds. Shake it. Presurrize more. Shake it. Pressurize it until it rock hard, all the while shaking strongly. You can get a really good swirling-shaking action going on with the stir bar inside of the unit. If you think about it, this is the principle that engineers use to package spray paints in such a way that the contents can be readily mixed, while being under pressure. I really cant emphasize enough the difference this made in my dream. Your shaking effort is actually reduced, while your mixing efficiency is exponentially increased. Shake some more.

I shook the unit vigorously, nonstop for two hours. Well, stopped every ten minutes to relieve gases, and purge. Squeeze it while holding the valve open,and purge two or three times. Away from your face. Have cold water nearby to immerse the unit in intermittently, while repressurizing. This improves uptake. Shake it. Shake it. See?

When you first place everything in the unit, the stuff is a light, green-brown-golden. It evolves to gold-brown, then brown, then brick-red at the end. Really hard shaking was used, and never let up on.

At the end, when it was brick red, I noticed a fine suspension of Pd particles. Then, would purge and add new air. The particles would go away for a short time and come back, so this was done a few times, and , evidently, as the reaction finished, the catalyst QUIT GOING BACK INTO SOLUTION and would deposit as a fine, granular silt on the sides of the SRV as you slowly rotate it.

The character of the solution seemed to change right about the time the shit went from brown to dark red, too. It seemed less viscous, and kinda acted like it was more easily agitated. I dont know how objective Im being here, just thiught I'd add that.

Remember, Shake It Real Hard. There were vertical cracks appearing in the unit at the end of the Rx, indicating that it was a hearty shaking affair, replete with purge and binge...

Make up dilute acid. Others have said that it's not needed, but in my dreams a much more efficient separation is achieved with dilute HCl being used to bust everything up. Hit the stuff with about 200-300 ml of this. It gets cloudy and tan-crap-greenish color and a HEAVY RED OIL falls out to the bottom. But its full of catalyst. Get the buchner funnel and your patience together. Assemble them. Filter all this crap about 3-4 times with the paper I have, don't know about you. A clear red oil is obtained, and believe it or not, ZERO TAR. ZERO.

The result? 37 ml of ketone from 50 ml safrole. Thats over 70%. Its repeatable. It IS NOT A FLUKE. There was extremely little iso and even less unconverted olefin. Removing the catalyst is a bitch, but its not really bad. You do need vaccuum. It seems like denatured ethanol is superior, in my dreams, to methanol as a substrate.

Well, there you have it. If anyone is not afraid of shaking for two hours, this is a very viable way to get the stuff.....

Low temps seem to favor a better all-round set of kinetics for this reaction.