Synthesis of Amphetamine from P2NP via SnCl2 and Zn

[yuiopjkl]

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

Spoiler: IMG 4

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.

Spoiler: IMG 12

 

[BlueDex]

Cool!

 

[TucoSalamanca.]

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

yuiopjklhow many ml of acetone do we use here

 

[yuiopjkl]

how many ml of acetone do we use here

TucoSalamanca.Until all the tin chloride is dissolved

 

[TucoSalamanca.]

36% hydrochloric acid

yuiopjklDo you have 37% hydrochloric acid?

 

[TucoSalamanca.]

Do you have 37% hydrochloric acid?

TucoSalamanca.can I use 37% hydrochloric acid here incorrectly translated

 

[yuiopjkl]

can I use 37% hydrochloric acid here incorrectly translated

TucoSalamanca.I think yes

 

[TucoSalamanca.]

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.

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

 

[TucoSalamanca.]

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

TucoSalamanca.?

 

[yuiopjkl]

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

TucoSalamanca.Yes

 

[blacky2340]

Why do you use dcm instead of other solvents?

 

[Bigballen]

I love you

 

[blacky2340]

I love you

BigballenI love you as well

 

[Bigballen]

I love you as well

blacky2340Now we must separate the dextroamphetamine and provide it to the masses! Godspeed

 

[Bigballen]

How much desired acid to add at the end?

 

[blacky2340]

How much desired acid to add at the end?

BigballenPour 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.

 

[Bigballen]

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.

blacky2340Would you know of other solvents that might be used instead of DCM?

 

[yuiopjkl]

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

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

 

[G.Patton]

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.

yuiopjklHello, 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]

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?

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

 

[TucoSalamanca.]

How many hours will we cool the sodium hydroxide solution?

 

[yuiopjkl]

How many hours will we cool the sodium hydroxide solution?

TucoSalamanca.Until it cools to room temperature