Síntesis de anfetamina a partir de P2NP mediante SnCl2 y Zn

yuiopjkl

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Comparado con la reducción de P2NP sobre amalgama de aluminio, este método ofrece una reacción significativamente más silenciosa (La reacción no es exotérmica ), mejor rendimiento (90%) y una sustancia muy pura (no requiere purificación adicional).

Disolver 15 g de P2N0 en 50 ml de acetona anhidra.
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Colocar un matraz de fondo redondo de 100 ml sobre un agitador magnético equipado con un refrigerante de reflujo. Añadir acetona y 42 g de cloruro de estaño(II) dihidratado.
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Enciende la agitación, espera a que se disuelva el cloruro de estaño y añade la solución de P2NP en acetona
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Agitar durante 20 minutos, la temperatura aumenta lentamente. Una disminución de la temperatura de la mezcla indica el final de la reacción. Poner 150 ml de agua fría y 4 ml de ácido clorhídrico al 36% en un vaso, añadir lentamente a la mezcla agitando. El color de la solución cambia
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Prepara una solución de hidróxido sódico (200 g por 200 ml de agua), enfríala a temperatura ambiente y añádela a la mezcla a pH>10 (en un medio ácido o neutro, la extracción de oxima es imposible), inmediatamente se forma un precipitado de sales inorgánicas.
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Extraer 3 porciones de 50 ml de acetato de etilo. Secar con sulfato de magnesio anhidro. Colocar 60 ml de ácido acético glacial en un vaso de precipitados sobre un agitador magnético y añadir la solución obtenida anteriormente (oxima en acetato de etilo).
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Mientras se agita, añadir 10 g de polvo de zinc.
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Remover durante 15 minutos.
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Añadir una solución enfriada de hidróxido de sodio (50 g en 100 ml de agua) hasta pH>10.

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Filtrar la mezcla. Añadir 50 ml de diclorometano, separar la capa orgánica y extraer adicionalmente la capa acuosa 3 veces con 20 ml de DCM.
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Se combinan los extractos orgánicos y se secan sobre sulfato de magnesio anhidro.
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Obtenemos una solución de 10 g de anfetamina base en DCM. Añadimos 50 ml de acetona anhidra y el ácido deseado para obtener la sal correspondiente.
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BlueDex

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¡Genial!
 

TucoSalamanca.

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cuántos ml de acetona utilizamos aquí
 

yuiopjkl

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Hasta que se disuelva todo el cloruro de estaño
 

TucoSalamanca.

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¿Tiene ácido clorhídrico al 37%?
 

TucoSalamanca.

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can I use 37% hydrochloric acid aquí traducido incorrectamente
 

yuiopjkl

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Creo que sí
 

TucoSalamanca.

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Entonces, ¿preparamos una solución de 200 ml de agua y 200 g de hidróxido de sodio y la añadimos aquí?
 

blacky2340

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¿Por qué utilizar dcm en lugar de otros disolventes?
 

waltjr5858

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Dcm is awesome and boils off super low... I'll use the or hexane. Toulene... too high more heat and work
 

Bigballen

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Te quiero
 

Bigballen

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¿Cuánto ácido deseado hay que añadir al final?
 

blacky2340

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Vierta 10 ml de acetona en 1 ml de ácido sulfúrico concentrado al 97%+ en proporción 10:1. Utilice una pipeta o una jeringa para dejar caer la solución lentamente hasta alcanzar un pH de 5,5. Si se sobreacidifica, añadir más freebase, si se sobreacidifica mucho y se convierte en líquido entonces a a/b y recristalizar.
 
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Bigballen

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¿Conoce otros disolventes que puedan utilizarse en lugar del DCM?
 

yuiopjkl

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Puede utilizar un disolvente no polar (éter, benceno, tolueno)
 

ActionAyi

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Yo también he pensado en el touleno, pero creo que la diferencia de densidad es demasiado baja, ¿no?
 

G.Patton

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Hola, ¡gracias por su informe! Es realmente interesante. 10g de base libre de amf es un rendimiento del 80,4%, bastante bueno. ¿Cuánta sal obtuviste?
 

yuiopjkl

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El método se copió de Internet.
Tengo previsto hacerlo en un futuro próximo.
Le avisaré cuando lo haga.
 

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 )
 

binkley78

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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
 

TucoSalamanca.

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¿Cuántas horas enfriaremos la solución de hidróxido de sodio?
 

yuiopjkl

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Hasta que se enfríe a temperatura ambiente
 
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