Amphetamine Sulfate

icecool · Insistent Chemist

Another problem occured, well a lot of them occur but they might also be usefull for people who might walk on to these problems once they are going to try this synthesis.
SWIM added ether to the mixture of Al/Hg/amphetamine freebase.
And there aren't any layers forming.
He added 20ml to 900ml mixture.
IIRC indole sayd once that per 100ml 10ml ether dissolves.
That means you would nee fucking much ether since ether is quite expensive...
Anyway SWIM will seperate the sludge from the nice light yellow layer and extract the yellow layer with DCM and the sludge with ether.

icecool · Insistent Chemist

SWIM just did an acid/base extraction on the freebase...
The freebase was dissolved in ether, he added HCl (1mol/L) 150ml to it.
And then let it settle, and got rid of the ether and then added DCM and the DCM turned pink and got rid of the DCM, then added NaOH (1 mol/L) 150ml and now there are these white fluffy crystals NaCl I suppose.
But there isn't an oil floating on top...how come?
And I added more water to get rid of these crystals but they won't go away they just keep floating threw the whole mixture.
Could it be that I don't see the oil since it is very pure now and waterlike color?
I started off with a slightly yellow ether extract...
SWIM filtered off these crystals and now he has a lighter DCM extract as what he started with.
This was his first succesfull a/b extraction so he's quite happy now.
He will tomorrow drain off the DCM layer so it can settle over night good.
Then dry it and then rotavap of the solvent and see what color the freebase is.

Thanks in advance!

IndoleAmine · Dreamreader Deluxe

icecool · Insistent Chemist

Aah fuck I added HCl so now I added DCM to the acidic layer and threw that away Crying or Very sad

I still do see some freebase (probably it is freebase).
After evaporating the solvent.
Anyway it was only a 8,5g P2NP reduction.
SWIM did add HCl during this reduction together with GAA so there would be more acid present though.
It isn't that much freebase though guess that is because of that wash with HCl and DCM...
I don't quite get that part about adding NaOH until cloudiness persist...
And well could you explain that part in a little more detail.

IndoleAmine · Dreamreader Deluxe

At the beginning, you have a clean waterlike acidic amine solution after washing with DCM.

(you can also back-extract the combined DCM washes with a little H2O and add this to the amine solution again, if you're afraid that some amine salt made it into the DCM washes)

Now you prepare a not too strong NaOH solution (20-25%), and add it slowly with good mixing, I would suggest to add it in small amounts, then swirl thoroughly each time afterwards.

At some point, you will see that adding NaOH causes something to happen: the solution turns white and cloudy, but this redissolves immediately when you mix the thing.

Now its time to be even more careful with adding NaOH in smaller amounts, until the white coloration doesn't redissolve anymore but stays. Now you have basified the solution, and can add nonpolar.

Then you should shake thoroughly to mix the np with the solution (this removes most of the white coloration, while the np becomes yellowish), THEN you can add more NaOH solution and watch those white coloration to re-appear each time you add some. You should shake after each NaOH addition at this point.

When further NaOH addition doesn't cause any more white coloration, it is finished. The pH is above 14, nothing will crash out anymore if you add more.

(BTW the white stuff is an emulsion of amine freebase and H2O; if you wait you can watch it form tiny droplets of oily substance floating to the top, and finally forming a small top layer of pure amine)

If you add too much NaOH at once, you could have problems with proper extraction, dunno why but it is harder if you add all NaOH at once, and advised to add it in small increments and to give the amine time to properly separate from the salt solution before adding more base and freeing more amine....

hope this helps.

i_a

icecool · Insistent Chemist

By the way for the people who don't already know this.
You should really pour acetone together with the filtrate and shut off the vacuum while filtering.
Then stirr the crystals up with the anhydrous acetone and then suck the acetone off and do this aprox 3 times.
Until the acetone comes threw clean.
If you didn't do that you might get brown/purple/pink amphetamine sulfate.
Not a problem either you can add anhydrous acetone to the crystals and then boil it for a couple of minutes and then let it settle (takes around a half a day) in the freezer so even less will be dissolved in the acetone if any does...
And then decant off the acetone ( I suck it up with a little pipette is more acurate IME). do this until the acetone remains clear.
Anyway this info I got thanks to indole_amine and it works great!
Got nice snow-white crystals now insted of brown/pink/purple what ever color.

SWIM got from 5,000g P2NP => 1,790g amphetamine sulfate.
Is this a normal yield?