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V primerjavi z redukcijo P2NP na aluminijevem amalgamu ta metoda ponuja bistveno mirnejšo reakcijo (Reakcija ni eksotermna ), boljši izkoristek (90 %) in zelo čisto snov (dodatno čiščenje ni potrebno).
15 g P2N0 raztopimo v 50 ml brezvodnega acetona
V NADALJEVANJU JE TREBARAZTOPINE RAZTOPITI.
100 ml bučko z okroglim dnom postavimo na magnetno mešalo, opremljeno s povratnim hladilnikom. Dodamo aceton in 42 g dihidrata kositrovega(II) klorida
Vključite mešanje, počakajte, da se kositrov klorid raztopi, in dodajte raztopino P2NP v acetonu
Mešamo 20 minut, temperatura se počasi dviguje. Znižanje temperature mešanice pomeni konec reakcije. V kozarec damo 150 ml hladne vode in 4 ml 36% klorovodikove kisline, ki jo med mešanjem počasi dodajamo zmesi. Barva raztopine se spremeni
Pripravimo raztopino natrijevega hidroksida (200 g na 200 ml vode), jo ohladimo na sobno temperaturo in dodamo zmesi do pH>10 (v kislem ali nevtralnem okolju je ekstrakcija oksima nemogoča), takoj nastane oborina anorganskih soli.
Ekstrakcija 3 x 50 ml porcij etil acetata. posušimo z brezvodnim magnezijevim sulfatom. V čašo z magnetnim mešalnikom damo 60 ml ledene ocetne kisline in dodamo predhodno dobljeno raztopino (oksim v etil acetatu).
Med mešanjem dodamo 10 g cinkovega prahu.
Mešajte 15 minut.
Dodajte ohlajeno raztopino natrijevega hidroksida (50 g v 100 ml vode) do pH>10.
Mešanico filtriramo, dodamo 50 ml diklorometana, ločimo organsko plast in dodatno 3-krat ekstrahiramo vodno plast z 20 ml DCM.
Organski ekstrakti se združijo in posušijo nad brezvodnim magnezijevim sulfatom.
Dobimo raztopino 10 g amfetaminske baze v DCM. Dodamo 50 ml brezvodnega acetona in želeno kislino, da dobimo ustrezno sol.
Na 1 ml koncentrirane žveplove kisline v razmerju 10:1 nalijte 10 ml acetona. S pipeto ali brizgalko počasi kapljajte raztopino, dokler ne dosežete pH 5,5. Če je prekislinjena, dodajte več proste baze, če je močno prekislinjena in se spremeni v tekočino, potem v a/b in ponovno kristalizirajte.
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
I DID ONE MORE "GOD-MOVE" AFTER THIS SURPRISE RESULT:.....
I SUCCEEDED IN MODIFYING THE SYNTHESIS - AND DID A REDUCTIVE AMINATION
WITH REFINED P2P AND METHYLAMMONIUMACETATE (OR KIND OF)
IT YIELDED METHAMPHETAMINE RACEMATE.... VERY UNEXPECTED QUANTITY- QUALITY AS SAME AS THE USUAL NABH4 ROUTE I PREFERRED BEFORE...
IT WENT DOWN FROM Imine formation -[ACIDIFIED VARIANT]...... TO HYDROCHLORIDE OF SLIGHT PINK APPEARANCE OVER NIGHT !
-->AT ROOM TEMPERATURE<----
PLEASE dont be mad at me but i decided to keep specifics for myself**
it is a whole new approach to phenetylamine syntheses in general ....
CREDITS TO THIS COMMUNITY PRO INSTRUCTIONAL P2P PURIFICATION TUTORIALS / I WENT TROUGH THE HASSLE OF THE WHOLE WORKUP TECHNIQUES OF THE BB-gate wisdom ...
THE PHENYLACETONE I DERIVED BY : Fe/H+ --P2NP---> Phenyl-2-Propanone
**(exception 4 you, Patton ..i made a writeup , documenting specs etc. i think you get what these
synthesis-dynamic principles hold in value )
Well done tripped over a n fell into dreamland. Don't see how sharing it wld take money outta Ur pocket though. Isn't that the point of this joint to help people learn new things n say fuk U to j law n the system / war on drugs. U just fuelin the fire like the rest to line Ur own pockets n fuk every one else
