PNP's into amphetamines reduction on alu foil

MargaretThatcher · Mon Apr 04, 2005 5:13 am

From the link you referred to:

"Quicksilver, an accurate description for elemental mercury, holds an almost magical fascination. In 1998 two Arkansas teenagers found about 40 pounds of mercury in an abandoned factory. They dipped their hands in it, poured it on floors in their homes to see it bead and shimmer, and they handed it out in jars to other kids at school."

The exposure was rather more than just having a few ml in the same room.

Bumblebee · Mon Apr 04, 2005 6:49 am

edited:
My Mama told me early never erver to break any of these thermometers and if i did so i had to say it to her . I think Parents should teach their children what is poisonous and what not.
I thougt the Children were in school age (minimum 6years old...) and so they can know that Hg IS dangerous. yes and I have also children and those neither put the fingers into the plug socket nor they play around with rat poison or Hg. Kids who do that have just a lack of parental education.
this spam-post about darwinism is deleted.

MargaretThatcher · Tue Apr 05, 2005 2:37 am

Going back to the Fe/HCl on P2NPs earlier in the thread, the Chemistry Survival Guide ebook linked to in the ebooks thread has a nice preparation of flakes of electrolytic iron, as used by Shulgin. Reduced iron may give better yields, but pure electrolytic iron must be better than iron filings.

***************************************
In this cool procedure, you can learn how to make highly purified metals, and the foundations of electroplating.

Method 1: Preparation of flaked highly purified iron, zinc, nickel, gold, chromium, silver, cadmium, titanium, cobalt, or zirconium using an open cell, and dilute hydrochloric acid

(By-products from reaction: Hydrogen gas)

Materials:

1. 450 milliliters (15.2 fluid oz.) of cold water

3. 1 iron, zinc, nickel, gold, chromium, silver, cadmium, titanium, cobalt, or zirconium nail, rod, wire or similar objects ranging from 5 to 15 millimeters (0.19 inch to 0.59 inches) in diameter by 6 to 9 inches in length

2. 25 milliliters (0.84 fluid oz.) of concentrated hydrochloric acid

4. 1 graphite rod of 5 to 10 millimeters (0.19 inch to 0.39 inch)
in diameter, or graphite rods of 1/4th inch diameter by 6 to 12
inches in length

Summary: Highly purified flaked metals can be prepared by electrolyzing a dilute solution of hydrochloric acid utilizing a corresponding metal anode and a graphite cathode. The electrolysis is generally simple, and produces beautiful flakes of the desired metal.

Hazards: Use caution when handling hydrochloric acid, and avoid inhalation of the fumes. Extinguish all flames before carrying out
the procedure as hydrogen gas is evolved, and use proper ventilation.

Procedure:

Forming highly purified flaked metals

Set-up the apparatus as illustrated below, and then fill the cell with 450 milliliters (15.2 fluid oz.) of cold water, and then add in 25 milliliters (0.84 fluid oz.) of concentrated hydrochloric acid. Thereafter, turn on the magnetic stirrer, and then stir the mixture and then attach the power supply clamps to the corresponding electrodes, and electrolysis the mixture at 6 to 12 volt at 2 to 6 amp direct current. During the electrolysis, the hydrochloric acid will be consumed forming the corresponding water-soluble metal chloride. Within about 15 to 30 minutes of starting the electrolysis, highly purified corresponding metal begins to form around the cathode. At the same time, the corresponding metal anode will slowly corrode and disappear. Even though the hydrochloric acid gets consumed, the electrolyte does not need to be replaced over time, and the electrochemical reaction can go on as long as there is a corresponding metal anode. In this procedure, the cathode should be composed of a graphite rod of 5 to 10 millimeters (0.19 inch to 0.39 inch) in diameter, and graphite rods of 1/4th inch diameter by 6 to 12 inches in length are preferred. Continue the electrolysis as long as
necessary, and afterwards, the highly purified corresponding metal can be filtered-off, washed, and then dried in the usual manner. The metal anode can be composed of iron, zinc, nickel, gold, chromium, silver, cadmium, titanium, cobalt, or zirconium. Note: The metal anodes should be rods, nails or similar objects ranging from 5 to 15 millimeters (0.19 inch to 0.59 inches) in diameter by 6 to 9 inches in length.

IndoleAmine · Dreamreader Deluxe

brain · Linguist Extraordinaire

about 300g p2np (left) and 250g pnp on right... (recrystalizeed-recrystalization)

will try some more these reduction Wink

-increasing the pressure-will increas the yeld??

IndoleAmine · Dreamreader Deluxe

Most likely yes - but please be careful with operating pressurized hydrogen in glas vessels.... Shocked

(The pictures look like liquid P2NP still - is this the way of cleaning with H2O you mentioned? Or is the light yellow stuff solid and P2NP, and the red upper layer crap?)

i_a

brain · Linguist Extraordinaire

no, these time recrystalized from ipa (have some old ipa-had to use or throw away).

brain · Linguist Extraordinaire

hm tried with EtOH .... the yeld is higher-product purer !! but have to add 200 not 100 ml EtOH (like in recepie) because it was not liquid !! wery hard to control temp, and mix, then was some owerheats ! and yeld was 20% !!! with 200ml EtOH 87-90% and easier to control the temp !!
-just add the amalgam to flask-and right away add to cold water [waterbath]

-when doing amalgam in situ - he product was wery impure !! Hg salts - with p2np will get red polymer !! with will impureing the product and yeld will be 60% !!

64bandil · Busy Bee

I must say I had my doubts about this reduction method when i first read about it. Don't have that anymore!

The last reaction gave 85% amphetamine directly from P2NP. The first trial gave about 50%. After a few experiments, I have decided that the following tweaks where responsible for the boost in yield:

- Used denaturated 93% ethanol instead of IPA (to lower overall price)
- Used 80% acetic acid, which is available OTC in bulk here.
- Didn't add any additional water, aside from the water present in the solvents.
- Added all of the aluminium foil in one portion. Gave on heck of an exothermic reaction, which had to be cooled externally.

Once the reaction was over, the ethanol was removed by distillation. After removal of this, the reaction porrage was basified with a 50% sodium hydroxide soln. Once basic, the whole shebang was steam-distilled to give crystal clear amphetamine floating on top of water. The distillate was acidified, washed twice with DCM. Basification with solid NaOH, gave a yellow oil, which was extracted with DCM. The DCM was washed once with dH2O and brine. DCM stripped and amphetamine isolated.

10,0 g's P2NP gave 7,0 grammes om amphetamine freebase (85% molar yield).

If I hadn't done this myself I wouldnt have believed the SOB claiming these kinds of yields...

Regards
Bandil

brain · Linguist Extraordinaire

64bandil · Busy Bee

Let me rephrase what I said, to make it more clear:

150 mL 93% Ethanol is mixed with 125 mL 80% acetic acid. The phenyl-2-nitropropene (10.0 g) is then added and heated / stirred untill full dissolution (and yes - it IS soluble in this). Mercury salt is added, followed by the Aluminium foil.

...and empirical knowledge says i'm right. It will do the trick, and reduce that nitropropene Smile

Regards
Bandil

IndoleAmine · Dreamreader Deluxe

Wow, good work guys! Cool

Now I'm convinced too - 80% yield with using EtOH (2x the amount) and 80% GAA finally sounds worthwile dreaming....

Do you (brain) really think in-situ amalgamation makes some polymeric mess? With ketone Al/Hg reductions, this makes no difference IMO. Maybe you have some water-soluble impurities in your HgCl2, which are removed when you prepare the Al/Hg before adding it, but which are inside the flask if you amalgamate in situ..

And steam distillation is indeed very easy, and perfect for purifying amph.
Just remember that Hg will evolve toxic vapor, so don't steam distill directly from the rxn flask (or you will have some elemental Hg in your collector flask too), better extract the whole with toluene first, wash the toluene/amine phase with brine, then add loads of pH13 water (NaOH) and steam out the amine and toluene - gives ulta-pure product everytime, and if you collect the distillate in a separatory funnel containing some acidic H2O, you can also do a further a/b directly (simply separate crap/toluene, basify to pH13, extract amine) - or you can simply distill into dilute NaOH, separate the toluene/amine, wash and remove solvent - less work, and already gives much, much purer product (although I think a further a/b can never be wrong).... Wink

cheers

i_a

brain · Linguist Extraordinaire

heh,, Hg salts will kill p2np !! and that is fact !! also will dirt the product - when steam destiil - the red dirt is destilled to.
-also adding NaOH is critical-points overheat

yes i'm 100% sure Smile

that when i used EtOH - the yeld was 80% ... used also 80% acetic acid. -bot know also-tha EtOH or IPa isnt critical point of yeld ! but purity- i think (but dont know on 100% !! too little tests)

I soluble p2np in ethanol only,,, the adding 0f next 100ml of EtHO is not on start ! but in half way-reduction-when the mass is "thicky"- the it dont poin overheat

im using spectral pure Hg + analytical grade HNO3 ->to give HgNO3 -rest of acid destilled of under reduced pressure.

64bandil · Busy Bee

Brain>

I am having some problems interpreting your latest post. But as far as I see, we mostly agree. I don't doubt that hg salts will destroy some of the nitropropene. However, it's present in so small amounts that only a tiny part of the nitrostyrene gets ruined. I didn't get any red goo that distilled over with the steam. It was crystal clear after distillation.

IndoleAmine> The point of distilling before the separation, is making sure every amine molecule is squezed out of the reaction porrage. I find it hard to separate the organic layer from the aluminium sludge. the a/b workup is done after the distillation anyway, so the Hg gets washed away there...

Regards
Bandil

IndoleAmine · Dreamreader Deluxe

brain> maybe the small percentage of Si in your foil makes red tar? Or it could be the different impurities in different alcohols (your Hg(NO3)2 sounds clean Very Happy

)...
And I think you wanted to say that you dissolve p2np in 1x EtOH, start the rxn, and when it becomes sticky and gooey, you add another 1x EtOH and the exothermic rxn is controlled and becomes more stirrable - right?

bandil> Yep, I'm just paranoid about Hg vapors - in reality I distill directly from the ugly soup too, and then I wash the organics thoroughly with bicarb and brine and filter thru celite - just much quicker... (my rational sense just tells me it would be better for my health if I did it the other way round.. Sad

) ...but then again I'm incredibly LAZY sometimes Very Happy

, so I decide against separating Al sludge and toluene phases and opt for steam distilling, everytime I would do it... Laughing

And then I usually start cursing and swearing like a drunk sailor, everytime when it comes to cleaning the glassware, because I have to remove that Hg mirror from the inside of my condensor and claisen, brrr... Evil or Very Mad

i_a