i just did this synthesis successfully ! (i was very astonished, that it works, like described...!)
i used 1,7g P2NP
- created sncl2 sol. from h202 and conc HCL first, until total dissolution, quenched oxidizing agent w. Bisulfite.
- dissolved p2np in acetone / EtoH and brought solutions of sncl2/p2np-solvent together in 250ml RBF
vigourously stirred for 2hrs.
------SKIPPED OXIME ISOLATION !!!!! -----
instead gave antoher dash of conc. HCL in to the whole
and gave finely divided active-C powder a hydrogen absorber in to RM.
then three portions of Zn-dust were introduced in several heaps...with subsequent hcl/EtoH addition.
as the reagents were used up i gave a small am. of AcOH to the whole and let it further react out a 15mins.
- now i slowly alkalized to ph 12 (metal precipitates formed immediate and sank...no hassle in base extraction....did with xylene/pet.ether/naphta mixture (+a small emulsion preventing splash of 2-propanol , every extraction step...)
i pooled organic xtracts, washed them with conc.brine f. rocksalt....)
afterwards the washed org.phases were run trough fine filtering apparatus.
added a 100mls of H20 and then titrated with Hcl until ph 5,5 ~
the acidic solution was equiv. mixed with acetone / ethanol-2propanol
with concentration under stirring with surface vent.
then the pasty residue was further refined...
I OBTAINED almost 1,3g amph-hcl (hygroscopic but useable!)
so that is a fine well thought route to go, THANKS TO ORIGINAL MASTERMIND