PNP's into amphetamines reduction on alu foil

icecool · Insistent Chemist

Okay then I get it now.
One question remaining Very Happy

You sayd that the amine will be floating on top of the water why don't you just put the whole mixture in the seperatory funnel, since it is floating on top you can drain away the water layer and be left with freebase, no?

brain · Linguist Extraordinaire

in my opinion, the amine is floating, but not whole-some amine will dissolve in NaOH solution, eto yelded product.

IndoleAmine · Dreamreader Deluxe

Exactly. It is slightly soluble in H2O, and when you basify you have a very fine "emulsion" of amine droplets swimming in the water, which have to be extracted with a nonpolar solvent (in which the amine is far better soluble-> distribution coefficient C1 / C2 < 1; see "distribution proposition" by Nernst).

btw brain: is your HCl salt hygroscopic? Making it can be done; but handling it without letting it turn into a wet puddle is hard IME..

cHEERS

brain · Linguist Extraordinaire

yes, its hygroscopic, i hawe to keep it in jar with CaCl2 (inside).

icecool · Insistent Chemist

When steam distilling do you get rid of the alcohol.
And then basify the Al sludge and steam distill that and safe that and extract that?
Or how about that...

I guess that the right way is to dump the alcohol (no not dump safe it Laughing

and pour back in flask of precious alcohol).
And then the rest which is not alcohol will be basified heavily then steam distilled and then add more NaOH to distillate...?

IndoleAmine · Dreamreader Deluxe

Exactly. But the alcohol should be stored in a separate container for re-use, since it isn't pure (contains some GAA and H2O), but still well suited for this kind of reduction..

Got any results already? Smile

icecool · Insistent Chemist

Not yet, I didn't fell asleep anymore so I haven't talked to SWIM anymore.
Cause he always talks to me in my dreams...
There is a thick paste/cake in the bottom since all the solvent evaporated off.
At least not all but well it is such a thick cake so too losen it SWIM added KOH solution.
Should have been plain water right...
Anyway now SWIM guesses there is solvent+amine coming over and well when all the solvent is gone now SWIM will add even more water+KOH so that when all the Al is gone.
Steam distillation can begin and he will worry about this later how to get the freebase out of the solvent...since it won't be that much probably?

P.S SWIM just had a great idea, he just safed 700ml solvent, and now he is left with a little bit of solvent and a basified Al sludge which is almost all dissolved now.
When steam distilling no amine is in the solvent but in the Al crap.
So now SWIM could also proceed from the step of just extracting the freebase out of all this crap.
Insted out a lot of water...
Okay there is this sludge to deal with but hey, since SWIM now most likely fucked up by already now adding the KOH solution he can fix the problem by just extracting it "now" (or tomorrow) and he also saved 700ml solvent with it Laughing

SWIM just added in 3 portions in total 176g KOH.
And now there is a yellow oil floating on top of the light grey solution in the flask.
Some solvent is already coming over because of the heat.
And in the beginning when that just happened some clear oily drops fell on the solvent and then dissolved in it...
Pretty weird SWIM thinks he is going to throw that back into the big soup.
And wait for a reply from a pro here and then proceed...
Doesn't look bad at all that nice yellow oil on top though Laughing

Bumblebee · Wed Apr 27, 2005 7:57 am

where we have to live ( Wink

) Petroleum ether is a cheap nonpolar solvent, wich is sold somewhere.
It is very clean and usually used in extracting herbs. Its boiling point ranges from 30-60°C. I guess its fine for replacing the expensive and dangerous diethyl ether, isn´t it?
I extracted some Hash oil some years ago and remembered this as a really useful solvent, that evaporates off quickly even from an oily fatty mass at room temperature.

icecool · Insistent Chemist

After steam distilling for a bit.
The mixture isn't nice yellow anymore with orange layer on top.
Now it is dark yellow/greyisch and the oil layer on top is dark red now.... Crying or Very sad

brain · Linguist Extraordinaire

i done 2 tests today, one flask was cooling intensly, second-wasnt(was self-boiling)

-i didnt see the differences in yelds(2-3%) !! and in 2-nd flask, amph*sulphate - was eawen optically 'whiter' (litle bit).

I extract with ethyl ether, dry with MgSO4,,, ad acetone (dont ewaporate ether)... then afrer adding H2SO4, the amph*sulphate will be on bottom of flask !! when can be easly decanted !!! (whih cant be done with only-acetone!! - it hawe some physics explanation). washed with acetone and filtred (grawity) pure salt-whih dont have to be washed more.
-I used this tome strong orange (wery impure) crystals p2np (giwen me for free from friend~60g)...

-I used 150ml- 80% AA+ 33ml EtOH 95%,,, (widouth adding more water) - next, add 10g P2NP, soluble in this mixture (will solube in ~90%), next add Al-Hg...

After 10-20min, the reaction is dont reduce anymore-look like,,, but i holded it for about~40-80min. then almoust all Al was 'disolwed' ... and hawe to add-much less NaOH...

icecool · Insistent Chemist

Brain your method is a lot faster since you don't need to evaporate off the solvents etc.
But how do you know how much H2SO4 to add?

brain · Linguist Extraordinaire

i dont wont to do more HCl salt .. the better way will be phpsphate...

when i dont ewaporate ether, i add by drops h2so4, litle shake, the salt is on bottom ! and clear solution on top (wird-but tru)... and you can see when to stop-when no more precipate is forming... or stop adding when ph will be~6,9 (6,8 ) [on wet paper)-but i like adding till precipate dont form... -when i was ewapotaring ether-i could calculate-how much h2so4 i had to use.

-then i decant the ether-acetone solution (as much as i can) -destiil it (to separate ether from acetone-dry, and use again (or redestill)... the precipate is dried, chhopped, and washed with acetone (gravity filtrate).

icecool · Insistent Chemist

Hmm that will speed up the process quite a lot.
So in fact.
You just extract the amphetamine freebase from the whole Hg/Al soup.
And then add acetone to the freebase (can be almost any solvent I guess since you can also dilute the freebase with EtOH MeOH etc to preticipate the sulfate in or phosphate or whatever).
But isn't it so when no preticipate forms anymore everything will dissolve back.
And is it possible to keep a bit freebase dissolved in ether.
And add that when you added too much H2SO4 solution in acetone/EtOH/MeOH...
This wouldn't be that a bad idea at all....
Then you also don't need to decant off the solution and take the crystals out.
You can add until nothing forms and then when it dissolves add a bit freebase to compensate...

brain · Linguist Extraordinaire

no, no

i add to ether acetone, then add H2SO4->decant, cash with acetone precipate->mix filtrate with decanted solution, add more h2so4, decant and wash again,

-its not the best way, but if someone have amphetamine freebase less than 20g it can be done-and isnt as much difficult, but Ph checking is also good (you hawe to have uniwersal paper with Ph=7,0;6,9;6,8;6,9 [6,9-6,8] ... -just add paper to solution (makeing paper wet isnt good idea after all-the salt will hydrolisys)

icecool · Insistent Chemist

Isn't it bad to add concentrated H2SO4 directly to the mixture?
And I would rather add a bit freebase after the sulfate starts to dissolve again in the excess H2SO4.
So then there is excess freebase again and the crystals will come back again.
Anyway is this a good idea???
Now you do not need to evaporate off the ether.
And you just add H2SO4 very slowely until the crystals dissolve when adding 1 drop too much, then add a few drops freebase solution and be sure to safe enough before starting adding the H2SO4 and then you will do the progress a lot quicker...
Any comments,
No offence to your method brain which sounds on the first impression safer but if you safe some freebase it is okay too...right?