PNP's into amphetamines reduction on alu foil

icecool · Insistent Chemist

Ah okay thanks, I also read there was an antidote for Hg poisoning, what is that?
Not that I'm going to take it, if I think I have a poisoning I would go to the doctor and tell him I broke my Hg thermometer and I spilled it and got it on my skin etc.
Anyway I think I will add the NaOH to the mixture now it is now cold again and will see if it succeeded it is now 5 hours so I guess it will be fine now...

IndoleAmine · Dreamreader Deluxe

icecool · Insistent Chemist

I didn't use a beaker...
And well the spillage isn't mercury it is NaOH solution...
Anyway SWIM is now extracting the black mixture with ether...

IndoleAmine · Dreamreader Deluxe

Hm - NaOH isn't that dangerous, although you should avoid spillages with such corrosive substances too if possible.

But about the beaker: what about this?

MargaretThatcher · Thu Mar 31, 2005 6:26 am

I am not so sure about the danger of elemental mercury. This is not the thread to debate this in. Maybe we can discuss this in equipment. At room temp, Hg has a low vapor pressure. It is also not cummulative at low exposure levels. Organic mercury is the evil stuff. I also wonder how much elemental mercury can make it through a correct extraction. I recall an old Hive thread where someone tested and got parts per billion. You get more exposure from your fillings.

icecool · Insistent Chemist

The extract is now standing in SWIM's laboratory and waiting (MgSO4 takes 12 hours ISRC to completely dry a liquid) anyway it is light orange/pink when looking quickly at it it looks red but when going there closely it is light orange.
The extract from the previous reaction where the Al had already been reacted before it was added to the P2NP (the fucked up one probably).
That extract is much darker red.
This afternoon it should be better wetter in SWIM's place and he will put the two beakers outside and heat the beaker to 45*C to evaporate off the ether and see what color the amphetamine freebase oil has.
And of course how many grams it is.
I suppose SWIM will not have a lot of oil from the first reaction maybe even nothing.
And SWIM did 6 extractions from the 600ml mixture he poured 100ml in the seperatory funnel each time and extracted it with 20ml ether or so.
Shaken really hard.

icecool · Insistent Chemist

SWIM has got around 12ml of red liquid, while he only used 3,5g of P2NP.
And at 50*C there doesn't evaporate any ether anymore.
Now what?

EDIT: Now there is 8ml left and the other extract has been evaporated and is now a very viscous red oil.
The other extract isn't extracted that far but SWIM thinks if there is some other crap left that won't form a sulfate and this is to see if there will be any amphetamine at all.
Anyway SWIM will first test (with the succesfull reduction) the a quarter of the total volume with H2SO4 and the whole part with the other one...
And can you get fusy from the fumes of the amphetamine freebase.
SWIM is feeling really funny and has to laugh constantely and is a bit dizzy etc...

IndoleAmine · Dreamreader Deluxe

Well one thing after the other...

1) mercury

IndoleAmine · Dreamreader Deluxe

Or try dissolving the oil in a slight excess of dilute auquous H2SO4, then wash with ether until the ether remains clean, then basify again with conc. NaOH solution until the amine falls out as a white/yellowish oil again.

Then extract with ether, dry and proceed as usual.

Why am I telling you this? Because the oil you got is red and far too much, when compared to the amnt. of p2np you used. This means there is a lot of crap present in you oil. The easiest way to get rid of it is to perform an acid/base extraction (dissolve amine in acid to make the salt of it, extract organic impurities with solvent, basify to release the amine from its salt again, extract free amine, evaporate solvent to leave pure amine)...

cheers

i_a

icecool · Insistent Chemist

Well hey don't forget this is the first time SWIM ever made it...
Anyway he just added H2SO4 dissolved in IPA which was dried with MgSO4.
And guess what crystals formed (white).
At the end slightly pink but almost not noticable.
Anyway SWIM has now got amphetamine sulfate Very Happy

yay.
Soon when it is dried SWIM will weigh the amount.
It was more to just make it not to get a good yield etc.

IndoleAmine · Dreamreader Deluxe

Congrats!

One last thing before you start to dry your sulfate: if you think you should maybe wash it - do it now! It can become really WHITE, if you purify the freebase properly (too late in your case maybe) or if you wash the salt thoroughly.

To do this, just boil the sulfate in enough dry acetone to cover it well (and then a little bit more, say a finger high) for a couple of minutes - the acetone will take on a slightly dirty coloration. Decant the acetone as good as possible, and repeat with fresh acetone until the solvent doesn't become colored anymore. Now filter off, and let air dry under a shining 60W light bulb (to provide very gentle heat) or preferably under a (infrared) heat lamp, a hotplate adjusted to 50°C (not more!) will work too.
If you did correctly, the salt will remain bright white until it is bone-dry powder, if you have impurities present, it will probably become yellowish on drying.

Enjoy your success, and not forget to dispose of the evil sulfate salt properly, by flushing it down the drain!

i_a

icecool · Insistent Chemist

Of course SWIM'll dispose of that f*cking life threatning sulfate properly.
SWIM'll completely distroy it first with 99% HNO3 and 98% H2SO4 and then with conc. NaOH etc.
and then flush it down the drain Wink

Anyway SWIM is enjoying his succes very much SWIM is walking around whole day with a big smile on his face.
And tomorrow is a new day and the whole house of SWIM stincks like ether, IPA etc now.
And SWIM's mother is not happy that is why he is going to build a fumehood, he already found a sparkless ventilator though Wink

.
And he will make a cabine out of plexiglass.
And also a hole in the side so when the distillation setup is standing next to the fumehood he can lead the vacuum adapter piece tube (lol) to the fume hood and so the fumes will get sucked away and so disapear out of the window.
And for other reactions he will make it like this so that the heating mantle will fit in the cabine completely and that a 1liter RBF fits in there with the condenser attached to it for reflux.
It won't get wider and higher then that.
And of course he will leave some extra space but on average it is going to be like that size.
And he will not make a thing like a real fume hood so you can slide the window up and down but has more something like a door in mind that is A LOT easier.
And swim read the whole improvised fume hood already just so you know...
And tomorrow he will clean all the glasswear because it is a total mess in SWIM's room/laboratory now.
And everything stinks like ether because there is ether sitting in everything etc.
And when he is going to clean that in the bathroom the half of the house is smelling like ether and his mother will get pissed again and blabla.
Anyway he will do the purification of the powder tomorrow or so...
And weigh the yield soon (it is now drying at room temperature).
SWIM wasn't able to measure how much freebase amphetamine there was because of several reasons:
SWIM didn't know when all the solvent had evaporated off...
The ether was all gone which boiled at 42*C insted of 36,4*C and at 50*C something was evaporating not noticable but after a while some liquid was gone but it was not boiling or fumes...
The scale that is acurate only weighs up to 50g and the beaker where it was in was more then 50g on it's own.
And the first reduction gave a really sticky red oil like substance, which dissolved more difficult then the second reduction did.
SWIM did the H2SO4 adding to 8ml of red liquid, it wasn't smelling like ether but it did have a smell which SWIM recognised but couldn't place the smell.
The first reduction gave white powder but that already dissolved again (probably because only a few drops of H2SO4 were already too much) the second one went better and SWIM added some and filtrated it (quite difficult though the filter got cloged up with crystals) and well adding more H2SO4 to the filtrate didn't give enough powder to it be usefull to filtrate again...
So to see SWIM added just enough in the first time...

EDIT: just posted this message/post and now SWIM noticed that he uses a lot the word "And" on almost every new line there is the word And in the beginning of the sentence...

IndoleAmine · Dreamreader Deluxe

MargaretThatcher · Sat Apr 02, 2005 4:07 am

Indoleamine: Wrt mercury. I appreciate your safety concerns and careless use of mercury could contaminate a building, but I think the exposure concerns are exaggerated. With dental fillings, elemental mercury is released from the dental alloy just by chewing. The people at real risk from drilling fillings are dentists, not the patient. If you swallowed 100 g of mercury, it would all come out of the other end; you would absorb some, but not enough to cause mercury poisoning. In the Middle Ages, drinking a few pounds of mercury was the standard treatment for a twisted bowel (kill or cure, and this tradition has continued with the British NHS). I was investigating this very topic last year, and the exposue rate from a few drops of mercury being open to the air in a normal room would not be cause for concern. Firstly, most rooms have air changes faster than every 8 hours, secondly, a few drops would not produce significant vapour, and thirdly, the safety levels for mercury vapour are very cautious. Also, people do excrete mercury through the kidney, bowl, skin and hair. Interestingly, there is some research that autistic children have much reduced mercury in the hair, suggesting that they cannot excrete it as efficiently.

So: yes, mercury should be managed and disposed of properly; no, elemental mercury is not as dangerous as the authorities make out; mercury salts and organo-mercury are a different matter - deadly.

Maybe we can stick together something about handling mercury for the equipment forum. I have a few bits and pieces on this.

Edited for spelling

IndoleAmine · Dreamreader Deluxe