Syntese af amfetamin fra P2NP via SnCl2 og Zn

yuiopjkl

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I6kJaAKTeX

Sammenlignet med reduktionen af P2NP på aluminiumamalgam giver denne metode en betydeligt roligere reaktion (reaktionen er ikke eksoterm), bedre udbytte (90 %) og et meget rent stof (ingen yderligere oprensning nødvendig).

Opløs 15 g P2N0 i 50 ml vandfri acetone.
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Anbring en 100 ml rundbundet kolbe på en magnetomrører udstyret med en tilbagesvalingskondensator. Tilsæt acetone og 42 g tin(II)chloriddihydrat.
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Tænd for omrøringen, vent på, at tinkloridet opløses, og tilsæt opløsningen af P2NP i acetone.
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Rør rundt i 20 minutter, og temperaturen stiger langsomt. Et fald i blandingens temperatur indikerer, at reaktionen er slut. Anbring 150 ml koldt vand og 4 ml 36% saltsyre i et glas, og tilsæt langsomt til blandingen under omrøring. Farven på opløsningen ændres
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Forbered en opløsning af natriumhydroxid (200 g pr. 200 ml vand), afkøl den til stuetemperatur og tilsæt til blandingen til pH>10 (i et surt eller neutralt miljø er ekstraktion af oxim umulig), der dannes straks et bundfald af uorganiske salte.
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Ekstraher 3 x 50 ml portioner ethylacetat. tør med vandfrit magnesiumsulfat. Anbring 60 ml iseddikesyre i et bægerglas på en magnetomrører, og tilsæt den tidligere opnåede opløsning (oxim i ethylacetat).
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Tilsæt 10 g zinkstøv under omrøring.
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Rør rundt i 15 minutter.
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Tilsæt en afkølet opløsning af natriumhydroxid (50 g i 100 ml vand) til pH>10.

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Filtrer blandingen. Tilsæt 50 ml dichlormethan, adskil det organiske lag, og ekstraher desuden det vandige lag 3 gange med 20 ml DCM.
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Organiske ekstrakter kombineres og tørres over vandfrit magnesiumsulfat.
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Vi får en opløsning af 10 g amfetaminbase i DCM. Tilsæt 50 ml vandfri acetone og den ønskede syre for at få det tilsvarende salt.
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BlueDex

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Det er fedt!
 

TucoSalamanca.

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Hvor mange ml acetone bruger vi her?
 

yuiopjkl

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Indtil al tinkloriden er opløst
 

TucoSalamanca.

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Har du 37 % saltsyre?
 

TucoSalamanca.

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Så skal vi lave en opløsning af 200 ml vand og 200 g natriumhydroxid og tilsætte den her?
 

yuiopjkl

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Ja, det gør jeg.
 

blacky2340

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Hvorfor bruger du dcm i stedet for andre opløsningsmidler?
 

Bigballen

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Jeg elsker dig
 

Bigballen

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Hvor meget syre skal der tilsættes til sidst?
 

blacky2340

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Hæld 10 ml acetone på 1 ml koncentreret 97%+ svovlsyre i forholdet 10:1. Brug en pipette eller sprøjte til at dryppe opløsningen langsomt ned, indtil pH 5,5 er nået. Hvis den er oversyret, tilsættes mere freebase, hvis den er meget oversyret og bliver til væske, tilsættes a/b og omkrystalliseres.
 
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Bigballen

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Kender du til andre opløsningsmidler, der kan bruges i stedet for DCM?
 

yuiopjkl

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Du kan bruge et upolært opløsningsmiddel (ether, benzen, toluen)
 

ActionAyi

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Jeg har også tænkt på toulen, men jeg tror, at forskellen i densitet er for lav, er den ikke?
 

G.Patton

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Hej, tak for din rapport! Den er virkelig interessant. 10 g amph-fri base giver 80,4 % udbytte, hvilket er ret godt. Hvor meget salt fik du?
 

yuiopjkl

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Metoden blev kopieret fra internettet.
Jeg planlægger at gøre det i den nærmeste fremtid.
Jeg giver besked, når jeg har gjort det.
 

Eleusius_hive_reboot

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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
 

Eleusius_hive_reboot

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* MAJOR ! update:...

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 )
 

TucoSalamanca.

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Hvor mange timer skal vi køle natriumhydroxidopløsningen?
 

yuiopjkl

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Indtil det er kølet ned til stuetemperatur
 
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