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Synthesis of Amphetamine from P2NP via SnCl2 and Zn

Bigballen

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How much desired acid to add at the end?
 

blacky2340

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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.
 

mithyl2

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how much anhydrous magnesium sulfate should be added at the stage when drying the ethyl acetate and just before adding the glacial acetic acid?
 

TucoSalamanca.

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how much anhydrous magnesium sulfate should be added at the stage when drying the ethyl acetate and just before adding the glacial acetic acid?
mithyl2I think you can stop adding magnesium sulphate when you realise that it is completely absorbed.
 

mithyl2

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At the stage before you add the DCM, do you separate the solution at all? (Because at the point just before you add the DCM you have the organic layer and the aqueous layer). Or do you add the DCM to the solution without the 2 layers being separated?

I just tried to separate the 2 layers and add DCM to the aqueous layer to start with, and then a lot of precipitate just came out of nowhere. I separated the DCM from it, dried it, added the anhydrous acetone, and then the acid, but absolutely nothing precipitated.

I also added the DCM to the other (organic layer I think, which must be ethyl acetate) and the DCM appeared to dissolve into it and didn't appear to form any layer. Is this normal? (Although here I added a small amount of DCM to a much larger amount of the solution.)
 

TucoSalamanca.

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At the stage before you add the DCM, do you separate the solution at all? (Because at the point just before you add the DCM you have the organic layer and the aqueous layer). Or do you add the DCM to the solution without the 2 layers being separated?

I just tried to separate the 2 layers and add DCM to the aqueous layer to start with, and then a lot of precipitate just came out of nowhere. I separated the DCM from it, dried it, added the anhydrous acetone, and then the acid, but absolutely nothing precipitated.

I also added the DCM to the other (organic layer I think, which must be ethyl acetate) and the DCM appeared to dissolve into it and didn't appear to form any layer. Is this normal? (Although here I added a small amount of DCM to a much larger amount of the solution.)
mithyl2You separate 3 times with ethyl acetate before dcm, i.e. ethyl acetate is used instead of dcm in the 1st extraction and dcm in the 2nd extraction.
 

mithyl2

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You separate 3 times with ethyl acetate before dcm, i.e. ethyl acetate is used instead of dcm in the 1st extraction and dcm in the 2nd extraction.
TucoSalamanca.and the ethyl acetate and dcm extracts are combined just before drying them, and then doing precipitation with acid?
 

yuiopjkl

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At the stage before you add the DCM, do you separate the solution at all? (Because at the point just before you add the DCM you have the organic layer and the aqueous layer). Or do you add the DCM to the solution without the 2 layers being separated?

I just tried to separate the 2 layers and add DCM to the aqueous layer to start with, and then a lot of precipitate just came out of nowhere. I separated the DCM from it, dried it, added the anhydrous acetone, and then the acid, but absolutely nothing precipitated.

I also added the DCM to the other (organic layer I think, which must be ethyl acetate) and the DCM appeared to dissolve into it and didn't appear to form any layer. Is this normal? (Although here I added a small amount of DCM to a much larger amount of the solution.)
mithyl2I don't understand your problem
At the stage before you add the DCM, do you separate the solution at all? (Because at the point just before you add the DCM you have the organic layer and the aqueous layer). Or do you add the DCM to the solution without the 2 layers being separated?
I think there is no difference.
The pH of the mixture must be 11-12.
The DCM layer is the bottom layer.
added the anhydrous acetone, and then the acid, but absolutely nothing precipitated.
I think it is better to evaporate the DCM and then add acetone to the amphetamine base.
I also added the DCM to the other (organic layer I think, which must be ethyl acetate) and the DCM appeared to dissolve into it and didn't appear to form any layer. Is this normal?
Why do you still have the ethyl acetate and oxime solution?!!
Yes, there will be no layers because DCM is miscible with ethyl acetate.
and the ethyl acetate and dcm extracts are combined just before drying them, and then doing precipitation with acid?
No!
Place 60 ml glacial acetic acid in a beaker on a magnetic stirrer and add the solution that previously obtained (oxime in ethyl acetate).
 

mithyl2

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I don't understand your problem

I think there is no difference.
The pH of the mixture must be 11-12.
The DCM layer is the bottom layer.

I think it is better to evaporate the DCM and then add acetone to the amphetamine base.

Why do you still have the ethyl acetate and oxime solution?!!
Yes, there will be no layers because DCM is miscible with ethyl acetate.

No!
yuiopjklAt step 10, when you are you filtering the mixture, do you want the NaOH layer separated from the ethyl acetate layer? Then you extract the oxime from the NaOH solution with DCM?

Because I thought the filtering at step 10 was only to get rid of the zinc, so you would still be left with the ethyl acetate layer and the NaOH layer, then you add DCM to these 2 layers, giving you 3 layers in total.
 

mithyl2

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Could someone also advise on if it's ok to use the hemihydrate form of the tin (II) chloride instead of the dihydrate?
 
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