PNP's into amphetamines reduction on alu foil

icecool · Insistent Chemist

SWIM now made 5 layer thick Al foil, and crumbled those squares up like in the pictures posted by brain but then the squares crumbled up.
And SWIM will use water and 35mg HgCl2 like tetraeder posted SWIM's method is just the method of tetraeder but then adjusted the amounts for his amounts.
So 3,5g P2NP; 5g Al foil, 35mg HgCl2 and 325ml of water.
Then let it react until Al gets darker and the mixture becomes gray and tiny bubbles start to evolve (before big bubbles started to evolve the reaction heated up until 55*C and was smoking quite a lot of H2 gas...)
Now he will wash the Al soon enough...

brain · Linguist Extraordinaire

gaa/ipa? can it be substitued?? gaa/etoh -what else??? [gaa-?]

icecool · Insistent Chemist

What do you mean brain?
Is that refering to my post or indole's post?
Anyway I've seen a lot of HgCl2 amalgamation reactions which use water as a solvent and only the P2NP needs to be dissolved in the IPA/GAA...

brain · Linguist Extraordinaire

so-did you add some ipa/gaa -in your post you didnt mention that Smile

icecool · Insistent Chemist

SWIM only did the amalgamation and there he didn't use any GAA/IPA
SWIM followed the same method as tetraeder in the first post of this topic only adjusted amounts for 7g P2NP anyway now he will do 3,5g P2NP.
And use 5g Al foil and 300ml hot water and 150mg HgCl2.
And he now knows what the problem was with the previous amalgamation he used 650mg insted of 65mg...

brain · Linguist Extraordinaire

hm,,, is addition ipa/gaa really nececery?? ... the p2np wil melt ;] and reduce quite nice??? or mabey the ipa/gaa is important for different reasons than disolving the p2np?

icecool · Insistent Chemist

SWIM just finised the reaction and everything.
Quite an intense chemical night so to say.
Anyway the amalgamation ...
The aluminium foil was 4-5 layers thick they were squares and then the squares were crumbled up to balls not hard pressed.
And then there was added to 5g of Al foil, 200ml of hot water 50*C and 100,0mg HgCl2 and it started to become gray the water and the aluminium started to evolve hydrogen gas.
After 7 minutes the aluminium contained very little black spots and it wasn't shiny anymore.
So SWIM decanted of the water washed the crumbles with 2x 200ml fresh and roomtemp water and the crumbles remained giving off hydrogen gas and making this funny noise, and slowely giving of more and more H2 gas and heating up.
Anyway then 60ml GAA and 40ml IPA were mixed and warmed up a bit to dissolve 3,55g of P2NP in it.
Then it was all added at once to the crumbles in a 500 ml RBF (in the meantime the crumbles almost didn't make a funny noise anymore and the flask wasn't hot anymore).
After a minute when the mixture of P2NP was added the flask heated up a little bit.
And to start the reaction the RBF was put in a heating mantle, and SWIM started to heat and heat and eventually at 80*C the IPA started to reflux and started boiling gently (really smootly).
The mixture became grey and the Al crumbles didn't dissolve as stated...
But some did but not much, and then after a while 20 minutes or so the mixture was quite thick and it was more like a beige/grey/white color.
And then NaOH solution was added to the stil hot mixture of Al sludge and it evolved some H2 gas the Al became shiny again and the mixture turned black slowely.
All the Al is now dissolved and tomorrow SWIM will extract the amph oil from the mixture with 3x30ml ether.
Anyway he doesn't know if it succeeded but he hopes it did ofcourse.
He will then dry the ether+oil with MgSO4 and then after 12 hours of drying, filtrate the MgSO4 off and let the ether evaporate off and measure the yield.

IndoleAmine · Dreamreader Deluxe

icecool · Insistent Chemist

Well SWIM now has an redish/orange oil which is dissolved in ether.
To the ether MgSO4 is added and when dry after 12 hours.
SWIM will let the ether evaporate and see if there is any oil left...
Anyway SWIM is quite confused now since you (indole) told me that when doing an Al/Hg reaction you should really first wash it with water etc.
And not do it like on rhodium a file is "photo assay on Al/Hg reduction of MDP2P...
So that is why SWIM perse wanted to wash it with water.
Well next time he won't wash the Al/Hg and just pour the mixture of P2NP/IPA/GAA right into the Al giving of hydrogen gas...
Anyway he will also use methanol insted of water then.
Pretty fucked up to waste 3,5g of P2NP (it's not much but when you only have 14g it is...)
Anyway I don't think everyones first Al/Hg reduction was a succes neither was the P2NP synthese.
So not that big of a problem, learn threw trial and error.
Now I also understand more about the Al/Hg reduction.
And well it was still hishing a bit but what the hell SWIM'll do it again.
Quite a lot of work fucked up yesterday.
But the whole procedure is the same as what SWIM has seen now exept next time there will really come a product out of it insted of probably a really shitty yield...

EDIT: Just noted long/large cubic crystals as clear as glass in the bottom of a beaker which contained Al/HgCl2/P2NP/IPA/GAA/water/NaOH
Everything together after the NaOH reacted with it.
That was still standing around and on the bottom there were these large needle like crystals...
Is this very pure P2NP which didn't react because the aluminium amalgam fucked up?
Picture:

brain · Linguist Extraordinaire

add water-if it soluble in water-its amphetamine*acetare >?
or will it be Al-salt..
---
can i extract amphetmaine freebase with xylene/toluene/benzene -dont evaporate! add some acetone, and H2SO40>will form crystals?

icecool · Insistent Chemist

They are soluable in water...
What else can I test if it is amphetamine.acetate, what would be the meltingpoint?
And would it be solvable in IPA, acetone, toluene, ethanol?
And what about the aluminiumsalt?

64bandil · Busy Bee

I would also bet on some aluminium salts. They ought to be soluble if enough water is present...

Try doing a marquis on them. If it turns too yellow - keep it Smile

icecool · Insistent Chemist

What is a marquis?

IndoleAmine · Dreamreader Deluxe

Marquis is a testing reagent for the presence of amphetamines, but I bet its no amph at all.

1) he basified the post-rxn mixture, extracted with Et2O - and used only a few grams of p2np, which would give a few grams of amph at most. After basifying and extracting, there shouldn't be such a large bunch of solid amph salt left - 0.5 grams maybe, but not this rather huge amount...

1b) if any salt was formed, it probably would've dissolved in the water unless he would've basified it completely, no? These one look as if they were grown in a saturated aequous solution, hard to accomplish with <5g amph and several hundred ml's of basic H2O.....

2) during basification, NaOH and GAA react to form sodium acetate - the biggest amnt. of substance that will be present after basifying usually is water, followed by salt.....

3) he already HAS some amine - where should all this molecules come from? (5g p2np used!!)

Maybe dissolve in water, basify to pH 15 with NaOH or better KOH, and see if anything falls out and if any amine smell evolves. Then you can extract it once more, but if not - discard. (if it were p2np, you would recognize it by the smell of amaretto I think)

cheers

i_a

icecool · Insistent Chemist

I think the P2NP got destroyed since you can destroy nitrocompounds with NaOH.
It also smelled like benzaldehyde after the reaction.
At this very moment SWIM is doing the amalgamation reaction again.
And he will trow in the solution of P2NP in 40ml IPA and 60ml GAA in the just started to amalgamating aluminium.
3,5g P2NP again 5g Al now and 70mg HgCl2 in methanol (175ml).
SWIM will pour all the P2NP solution in there all at once, that can't be bad with this small amounts right?