11-21-03 08:48
No 472180
To the hive collective,.
Are there any bees that have been successfull in making Pdcl2 from this method,....
Post 376913 (GOD: "Whats up with the PdCl2???", Chemicals & Equipment)
--It does work. to one troy ounce palladium coin is added 100ml nitric acid and 300ml HCl. Stirred occasionally with a glass rod, covered with parafilm. When fizzing stops, decant supernatant, brown chunk o' Pd will be at bottom of beaker. Add 100ml nitric and 300ml hydrochloric acid again. Once fizzing stops, decant. If any solids are left, which a few flakes will probably beeeee, add a little bit more aqua regia. Combine supernatants evaporated with occasional stirring and glass boiling beads. Once all liquid is evaporated, red-brown solid is left on hot plate for about .5hrs. Glass beads are removed and solid is powdered in mortar and pestle. Yield is always around 55-56g.
10g palladium something, 760g benzo, 2L methanol, 250ml water, 900g safrasomething. Reflux briefly and heat at 53-58C for 4-6hrs. Standard workup. Good vacuum source makes it drip, drip, drip at 105-110C in the claisen. Often it is blue in tint. Yield varies between 575-650g, not the greatest, but satisfactory.
Always have a problem with borohydride reduction. ~350g from 500g ketone, consistently. Achieved after distillation and a single recrystallization. Procedure from LT.
In Al/Hg, according to the scribe of MM, only scaled 3X, 58-61g recrystallized product, consistently.
Mr. and Mrs. Bioassay like it and notice no difference in the high compared to product made with different PdCl2(oh yeah, I forgot, I made something else).
Any help would be appreciated,
hoffman
(Hive Addict)
11-21-03 10:39
No 472210
evaporate and add HCl until no more evolution of NOX gasses are observed then procedd to evaporate.
Me wonders if the same can be done with conc. Hcl and Conc. H2O2 the mechanism in the aqua regia process involves nitriyl chloride NO2Cl this is basically free rad Chlorine would H2O2 and Hcl generate the same free rad chlorine to convert Pd (0) to Pd (II)???
(Stranger)
11-22-03 04:16
No 472390
Spisshack,
Thankyou, I am impressed here, at the response rate,
So what you are saying is that eventually, after using aqua regia, and a few subsequent hcl boils, and a final evapouration, everything should break down to pd(ii)cl2,
thankyou again
hoffman
(Hive Bee)
12-09-03 08:50
No 475587
I make all my PdCl2 this way. It works fine & my MM wackers have fairly decent yields (although I do use 2.5g of PdCl2). I can't subjectively compare yields however as I've never used anything but homemade PdCl2.
I've also read it's best to evap the Aqua Regia then add HCl & evap (& repeat maybe 3 or 4 times). I don't do it though.
I make all my HgCl2 the same way, however I've heard that this ends up in a mix of Hg2Cl2 & HgCl2. I believe it too as my MM Al/Hg's take a lot longer to begin aminating than he describes. I usually put in ~800mg of my homemade HgCl2.
Just be careful buying Nitric Acid.