palladium katalyst???

[BeeG]

18gr of Palladium on Carbon were prepared using following methode:


- 1,7gr PdCl2 in 2ml 31% HCl and 20ml dH2O are heated for 15min at 80°
- 20gr activated carbon are heated with 450ml H2O and 15ml 31% HCl for 2h;
the carbon is filtered off
- the PdCl2 solution is added to 30gr sodium acetat trihydrate in 200ml
dH2O in a 500ml Flask
- the washed carbon is added to this solution
- hydrogenate the mixture for 3h, using drone's hydrogen generator; set
it up to produce 1mol of H2; don't forget to stir vigorously; iron
powder works nicely (only powder works, sheet's won't)
- when the hydrogenation is complete and the carbon settles down and you
should have a colorless mixture with the catalyst at the bottom
- filter the carbon , wash it with 4-5*100ml dH2O; dry the catalyst at 50°
- I got 18gr (my filter methode wasn't good, use only glas no plastic,
easier to clean) of 5% Palladium on Carbon;


- - - - -


- 22gr highly purified Phenyl-2-nitropropene
- 300ml 99% glacial acetic acid (maybe too much)
- 38gr Ammonium Formate
- 9gr 5% Palladium on Carbon ( Pd-C)


were introduced in a 500ml Flask.


22gr P2NP were dissolved in 300ml 99% glacial acetic acid and added
to the 5% Pd-C. All was heated to 100° and vigorously stirred.
I introduced 3*~13gr Ammonium Formate; All was refluxed for 25 min;
Then everything was cooled; 100ml Chloroform were added so that it
is easier to filter the Pd-C. I used normal coffee filter paper and
vacuum, which worked. Then i added 1l of dH2O and the Chloroform
separated out. The layers were separated andi "washed" again with
additional 100ml Chloroform. But amphetamine wasn't soluble in the
glacial acetic acid, so i extracted it with the chloroform.


The chloroform was eliminated and i got 15.5gr of a yellow oil,
which was dissolved in 200ml 15% HCl, washed trhee time with 75ml
DCM, made basic with 25% NaOH and extracted with Ether. And again
i failed to make the HCl salt , i tried to dry the ether with Epsom
Salt and then to afford the salt with dry HCl. But all i got was a
slightly yellow colored layer at the bottom of my ether mixture.
I decided then to make the salt with 99% H2SO4 in Ether and Ethanol,
which worked perfectly. (first i made again everything basic...)
The salt was washed and i got 14gr of white! Amphetamine salt.


- - - - -


I didn't use any H2SO4 in the CTH because i don't know if it helps or if
it destroys everything, maybe it helps and the yields would be higher.
Maybe anhydrous ethanol works better, if anyone sends my Calcium oxide
POWDER i will try it )


Palladium on carbon is not easy to handle, i suggest to use only glas
filter funnels, my plastic funnel is still full with carbon.


Anyone knows a secure methode to form the HCl salt of an amphetamine ?
I dried with the Epsom Salt (~30gr) for 2h, is it not possible to dry
with Epsom Salt (MgSO4 * 7H2O)? already too many H2O's ?





so, my question is ...does anybody dreamed about this procedure??? And could swim use the catalyst many more times?? and could swim use the shame katalyst with only 10%palladium.....thats easy to get...5% i don´t sawEdited by: gerhard