Amfetamino sintezė iš P2NP naudojant SnCl2 ir Zn

yuiopjkl

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Palyginti su P2NP redukavimu ant aliuminio amalgamos, šis metodas užtikrina gerokai ramesnę reakciją (Reakcija nėra egzoterminė ), geresnę išeigą (90 %) ir labai gryną medžiagą (nereikalingas papildomas gryninimas).

Ištirpinkite 15 g P2N0 50 ml bevandenio acetono
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Ant magnetinės maišyklės su grįžtamuoju kondensatoriumi uždėkite 100 ml kolbą su apvaliu dugnu. Įpilkite acetono ir 42 g alavo(II) chlorido dihidrato
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Įjunkite maišymą, palaukite, kol alavo chloridas ištirps, ir įpilkite P2NP tirpalo acetone
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Maišykite 20 minučių, temperatūra kyla lėtai. Mišinio temperatūros sumažėjimas rodo reakcijos pabaigą. Į stiklinę įpilama 150 ml šalto vandens ir 4 ml 36 % druskos rūgšties, maišant lėtai įpilama į mišinį. Tirpalo spalva pasikeičia
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Paruoškite natrio hidroksido tirpalą (200 g 200 ml vandens), atvėsinkite jį iki kambario temperatūros ir įpilkite į mišinį iki pH>10 (rūgščioje ar neutralioje aplinkoje oksimo ekstrakcija neįmanoma), iš karto susidaro neorganinių druskų nuosėdos.
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Ekstrahavimas 3 x 50 ml porcijomis etilacetato. išdžiovinkite bevandeniu magnio sulfatu. Į stiklinę ant magnetinės maišyklės įpilkite 60 ml ledinės acto rūgšties ir įpilkite anksčiau gautą tirpalą (oksimą etilacetate).
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Maišant įberkite 10 g cinko dulkių.
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Maišykite 15 minučių.
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Įpilkite atvėsinto natrio hidroksido tirpalo (50 g 100 ml vandens), kad pH>10.

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Mišinys filtruojamas. įpilama 50 ml dichlormetano, atskiriamas organinis sluoksnis ir papildomai vandeninis sluoksnis ekstrahuojamas 3 kartus 20 ml DCM.
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Organiniai ekstraktai sujungti ir išdžiovinti virš bevandenio magnio sulfato.
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Gauname 10 g amfetamino bazės tirpalą DCM. Įpilkite 50 ml bevandenio acetono ir norimą rūgštį, kad gautumėte atitinkamą druską.
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BlueDex

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Šaunu!
 

TucoSalamanca.

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kiek ml acetono mes čia naudojame
 

yuiopjkl

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Kol ištirps visas alavo chloridas
 

TucoSalamanca.

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Ar turite 37 % druskos rūgšties?
 

TucoSalamanca.

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ar galiu naudoti 37% druskos rūgštį čia neteisingai išversta
 

yuiopjkl

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Manau, kad taip
 

TucoSalamanca.

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Taigi, ar paruošiame 200 ml vandens ir 200 g natrio hidroksido tirpalą ir jį čia įpilame?
 

blacky2340

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Kodėl vietoj kitų tirpiklių naudojate dcm?
 

Bigballen

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Aš tave myliu
 

Bigballen

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Kiek norimos rūgšties pridėti pabaigoje?
 

blacky2340

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10 ml acetono užpilkite 1 ml koncentruotos 97 % + sieros rūgšties santykiu 10:1. Pipete arba švirkštu lėtai lašinkite tirpalą, kol bus pasiektas pH 5,5. Jei per rūgštus, įpilkite daugiau laisvosios bazės, jei gerokai per rūgštus ir virsta skysčiu, tada į a/b ir pakartotinai kristalizuokite.
 
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Bigballen

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Ar žinote kitų tirpiklių, kurie galėtų būti naudojami vietoj DCM?
 

yuiopjkl

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Galite naudoti nepolinį tirpiklį (eterį, benzeną, tolueną)
 

ActionAyi

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Aš irgi galvojau apie tuleną, bet manau, kad tankio skirtumas yra per mažas, ar ne ?
 

G.Patton

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Sveiki, dėkojame už pranešimą! Jis tikrai įdomus. 10 g laisvosios amfo bazės yra 80,4 % išeiga, visai neblogai. Kiek druskos gavote?
 

yuiopjkl

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Metodas buvo nukopijuotas iš interneto.
Artimiausiu metu planuoju tai padaryti.
Pranešiu jums, kai tai padarysiu.
 

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 )
 

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Kiek valandų vėsinsime natrio hidroksido tirpalą?
 

yuiopjkl

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Kol atvės iki kambario temperatūros
 
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