Urushibura Ni catalyst

[Grignard]

is there anyone that have tryed the urushiba nickel reduction of PN2P? Could the deposited Ni after the reduction be reused after washing with acetone and HCl? Last time i was draming of this reduction the mixture smelled very amine but all i got eas a very thick red syrup, but i used a very dirty PN2P.. How is the possibillity for suksess in this raction??

[stratosphere]

the nickel could be reused by extracting the solid nickel, washing, then reforming a nickel salt.

i suppose NiS04 would form by putting it in concentrated sulphuric acid.(?)
but watch out for S02 if you use this method.

[Grignard]

Thank`s , so the percipitated Ni(s) cold not be used directly.. I dont understand the synthesis at rhodium, it say there will be two layers of water and alcohol/amine?? Is there a possibillity to over reduce the PN2P?

[stratosphere]

i don't know, but as i understand the hydrogen gets absorbed into the Ni as it gets reduced, so trying to reuse the nickel metal directly wouldn't work.

[Rhodium]

It's been done before by Ritter:

Urushibara Style Amphetamine

(https://www.thevespiary.org/rhodium/Rhodium/chemistry/amph.urushibara.html)

Amphetamine can not be reduced any further by Urushibara Nickel, at least not under the above conditions, so overreduction is not a problem (BTW, how did you arrive at the abbreviation PN2P?).

Alcohol and water are usually fully miscible, but if there are lots of salts dissolved in the water, a majority of the alcohol may separate and float on top of the aqueous salt solution. The alcoholic layer will contain almost all of the amphetamine at basic pH's, but you will ensure higher yields and a much purer product by working up as follows:

Extract the aqueous layer with diethyl ether (or equivalent) after decanting the alcoholic layer, mix it with the extract and evaporate the solvents. Dissolve the residue in 100 mL 5% HCl, wash once with 25 mL ether (discard), basify with aqueous NaOH and extract the amphetamine freebase with 3x20 mL ether, dry the solution over a little anhydrous MgSO₄, filter and evaporate to get relatively pure amphetamine freebase.

Crystallize by making either the sulfate, phosphate or oxalate salt as described elsewhere, as the hydrochloride is so  deliquescent (hygroscopic) that it's almost uncrystallizable, and it won't keep in air.

[Grignard]

Yeeees....  i think that will do it!! Thank`s everyone! I will try to extract the alcohol layer, Could the EtOH be substituted by MeOH or isopropyl alc? I used MeOH and it seems to be ok, but there was a som minor problems with the boiling point and the heat developed by the eksothermic addition of Al to the PN2P...

[Grignard]

I keep tryin this reduction, but all i seems to get out of it is a thick red oil/tar that sticks to everything! Hvat is this shit, and why is this happening? i use MeOH as a solvent, and follow the recipe! The PN2P i light yellow and seems to be very ok.... Is there another possibility than adding NaOH after all of the Al has reacted, because it smells very very amine until i add the NaOH, after that everything smells ammonia....

[Rhodium]

Have you used Ritters procedure, together with the iumprovements suggested in

Post 464850

(Rhodium: "Urushibara Style Amphetamine", Chemistry Discourse)? If you still experience problems, you may need to distill the freebase before crystallizing it. You can distill in any fashion you like, as the sturdy freebase can be purified by either steam distillation, vacuum distillation or even distillation at atmospherical pressure (bp ~200°C iirc).

[Grignard]

I have followed ritters method and the ekstraction you described, but there is nothing in the HCl layer. I got a lot of very bad smelling red oil. In the beginning of the reduction i saw that the mix got deep red but it changed to a grey thick mass smelling amine. Is there a possibillity to destill the thick grey mass directly by steam distillation?