Synthesis of Amphetamine from P2NP via SnCl2 and Zn

yuiopjkl

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Compared to the reduction of P2NP on aluminum amalgam, this method offers a significantly quieter reaction (The reaction isn't exothermic ), better yield (90%) and a very pure substance (no additional purification required).

Dissolve 15 g of P2N0 in 50 ml of anhydrous acetone
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Place 100 ml round-bottomed flask on a magnetic stirrer equipped with a reflux condenser. Add acetone and 42 g of tin(II) chloride dihydrate
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Turn on the stirring, wait for the tin chloride to dissolve and add the solution of P2NP in acetone
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Stir for 20 minutes, the temperature rises slowly. A decrease in the temperature of the mixture indicates the end of the reaction. Place 150 ml of cold water and 4 ml 36% hydrochloric acid in a glass, slowly add to the mixture with stirring. The color of the solution changes
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Prepare a solution of sodium hydroxide (200 g per 200 ml of water), cool it to room temperature and add to the mixture to pH>10 (in an acidic or neutral environment, extraction of oxime is impossible), a precipitate of inorganic salts immediately forms.
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Extract 3 x 50 ml portions of ethyl acetate. dry with anhydrous magnesium sulfate. Place 60 ml glacial acetic acid in a beaker on a magnetic stirrer and add the solution that previously obtained (oxime in ethyl acetate).
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While stirring, add 10 g of zinc dust.
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Stir for 15 minutes.
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Add a cooled solution of sodium hydroxide (50 g in 100 ml water) to pH>10.

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Filter the mixture. add 50 ml dichloromethane, separate the organic layer, and additionally extract the aqueous layer 3 times with 20 ml DCM.
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Organic extracts combined and dried over anhydrous magnesium sulfate.
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We get a solution of 10 g amphetamine base in DCM. Add 50 ml of anhydrous acetone and the desired acid to obtain the corresponding salt.
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BlueDex

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TucoSalamanca.

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how many ml of acetone do we use here
 

yuiopjkl

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Until all the tin chloride is dissolved
 

TucoSalamanca.

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Do you have 37% hydrochloric acid?
 

TucoSalamanca.

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So, do we prepare a solution of 200 ml of water and 200 g of sodium hydroxide and add it here?
 

blacky2340

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Why do you use dcm instead of other solvents?
 

Bigballen

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I love you
 

Bigballen

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How much desired acid to add at the end?
 

blacky2340

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Pour 10ml acetone onto 1ml concentrated 97%+ sulfuric acid 10:1 ratio. Use pipette or syringe to drop the solution slowly until pH 5.5 is reached. If overacidified, add more freebase, if way overacidified and turns into liquid then to a/b and recryistalize.
 
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Bigballen

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Would you know of other solvents that might be used instead of DCM?
 

yuiopjkl

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You can use a non-polar solvent (ether, benzene, toluene)
 

ActionAyi

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I have thought about toulene too but i think the difference of density is too low isnt it ?
 

G.Patton

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Hello, thank you for your report! It's really interesting. 10g of amph free base is 80.4% yield, quite good. How much salt did you get?
 

yuiopjkl

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The method was copied from the Internet.
I plan to do it in the near future.
I'll let you know when I do it.
 

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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How many hours will we cool the sodium hydroxide solution?
 
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