PNP's into amphetamines reduction on alu foil

IndoleAmine · Dreamreader Deluxe

Yes, pour'er in straight at once, but have a cold water bath at hand. You don't want mercury chloride/MeOH spillages...

i_a

icecool · Insistent Chemist

It isn't that spectaculair.
When the Al got dark dots and the hydrogen was bubling.
SWIM poured in the P2NP solution.
And now it heated up to a reflux.
But it isn't boiling heavily.
There also isn't a lot of hydrogen evolving.
could it be that the pieces of Al are too large it are 1" squares folded into nuggets (not shredded in the mixer).
They are just floating around in the methanol the color is grey/black now.
And it isn't heavy or anything at all...

IndoleAmine · Dreamreader Deluxe

Hey, sounds about right I think!

icecool · Insistent Chemist

You sure?
The Al isn't dissolving...
SWIM just put it on the magnetic stirrer and put it full blast so it is swirling like hell now.
Anyway there are little flitters of Al floating around which are shiny.
I only poured in big pieces of Al and now there are these tiny Al pieces.
Is this what I read in some posts the shiny things on surface?

IndoleAmine · Dreamreader Deluxe

Wait - you dumped in big pieces, now you have small pieces?

Why do you think it would not dissolve? (after only six minutes of waiting??)

I would say the size of the Al pieces becoming smaller is a sure indicator for the progress of their dissolution.... Very Happy

(be patient! Let stir for a couple hours, time is not money in your case I guess... maybe apply gentle heat with hot water bath, to speed up things a bit...)

i_a

icecool · Insistent Chemist

Okay well I do know that next time I'll put in smaller pieces.
Before hydrogen was bubbling like hell, and shouldn't the process take 20minutes or so.
What do you suspect this would take and when do I know it is finished when all Al is dissolved?
I poured in a bit extra HgCl2 so now in total there is in 100mg HgCl2.
60ml GAA, 40ml IPA; 3,5g P2NP, 175ml methanol and the temperature is now, 42*C.
And when should I apply extra heat, since I can't stir and heat at the same time...

EDIT: Just read what you edited and well shall I apply heat with heating mantle for a while and then stir again and so switch between the two of them?

IndoleAmine · Dreamreader Deluxe

icecool · Insistent Chemist

Okay I guess SWIM'll be fine I'll go and tell him in a couple of minutes.
And he also asked if there would be some Al that didn't react yet if that will later on? with the HgCl2...

IndoleAmine · Dreamreader Deluxe

icecool · Insistent Chemist

So practically if you use really big pieces of Al you can let it stir for a year.
And the reaction will go on.
But just very slowely.
SWIM told me that more Al had dissolved at least he thinks it did...

IndoleAmine · Dreamreader Deluxe

Exactly. If really big amounts of substrate are to be reduced, this is the way to avoid exothermic rxn becoming uncontrollable and making a nice vulcano - use Al sheets instead of foil, make the rxn slower and let it run longer instead.

But with 5g p2np, you could try using thinner foil next time (or fold it just 3x...)

i_a

icecool · Insistent Chemist

I'll tell SWIM to do that next time, you see he doesn't have a internet so I go and tell him every time via the phone, since he lives quite far away from me.
And well what he needs to know that is what I post and then I tell him again what the experts say.
Anyway he told me that the reaction now is quite dark and there is less Al foil left and he is now letting it heat for a while and then stirs for a while and so on.
The small Al pieces have dissolved now and I told him that in the picture assay which is on rhodium the color becomes grey/white after a couple of hours when all/almost all the Al has dissolved and then it will cool down.
And SWIM is just going to heat it nicely and let it stir away.
Anyway could it be bad for the chemicals that would for or anything to keep stirring all night long or weeks while the Al has all dissolved or when the reaction is finished?
And could it also be that a little bit of Al won't dissolve?
If you add more methanol will more Al dissolve?
The pieces of Al are now full of little black spots and the reaction is refluxing and blabla...
Quite funny though, he is not in his room because of the fumes, and he put a webcam on the reaction vessel and is sitting at another computer and watching his webcam via the network lol...

icecool · Insistent Chemist

Here are 2 pictures that SWIM send me via his phone...

This is seen from the top and it is the actual color, because with a flash it becomes gray while it is red that is just because the walls are slightly coated with the Al sludge...

Here is a picture of the side of the RBF and well not all the Al has dissolved yet.
But well what should SWIM do now it has been stirring and heating since 4 hours now...
So I guess SWIM should let it cool down now and just add the NaOH solution right?
IF it fails which SWIM doesn't think so he will do it again another time and use less thick Al foil so the reaction will be heavier...
But hey better the first time a slow reaction than a TOO heavy reaction where everything flies out of the RBF...
Very Happy

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P.S About the safety of HgCl2 of course Hg is never good for you.
But when doing reductions SWIM used 70mg.
And this information have I got:

Draize test, rabbit, eye: 50 ug/24H Severe;
Draize test, rabbit, skin: 500 mg/24H Severe;
Oraal, muis: LD50 = 6 mg/kg;
Oraal, rat: LD50 = 1 mg/kg;
Skin, rat: LD50 = 41 mg/kg;

I dunno what a draize test is, but when you look at orally what is lethal, 6mg per kg of body weight.
Let's say I weigh 70kg then 70x6mg would be lethal for me right...
And tested on a rat only 1mg per kg is enough so then when I would swallow ALL of the HgCl2 that I used THEN I could die because this is the lowest dose noted on when a animal died...
But I am never going to orally take all the 70mg of the HgCl2 used...
And threw the skin as seen by the rat 41mg per kg is deadly.
that means that I would need to absorb 2870mg of HgCl2 threw my skin to be dead...
SWIM told me he did had to cough a lot but he suppose that is just because he is sick of walking around in a t-shirt all day while it wasn't that warm outside...

Ionium · Wed Mar 30, 2005 10:18 pm

Don't forget the fact that Hg accumulates in the body. This means that if you use Hg-salts lets say 10 times a year, and you absorb just 1 mg each time, it will be doing considerable damage to your health after a few years. You should ALWAYS take necessary steps to prevent absorbtion of ANY amount of Hg-salt, to prevent both short-term and long-term damage.

IndoleAmine · Dreamreader Deluxe

This is the reason why fish is generally considered uneatable if it contains more than 0.05mg Hg/kg..... (EU standard; there are exceptions for certain kinds of fish though)

i_a