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cyberzed
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[edit]
[Edited on 8-1-08 by cyberzed]
[Edited on 8-1-08 by cyberzed]
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Nicodem
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Are you sure you did not confuse this forum with a certain other forum.
Anyway you are lucky no crystals precipitated at the end since otherwise you would have just wrote the admission of having broke the law since unless
you live on Antarctic continent you would be breaking the laws of your country. And I’m not even sure you would be safe from UN regulations on
Antarctica. If any crystals would precipitate, by al misfortune, they would be crystals of a compound illegal to manufacture and posses
practically al over the world.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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Organikum
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Here where I live I am allowed to do such things provided that I destroy the product immediately after identification and quantification.
You never know what may form in the end.
But in the writeup there are to many possible points of failure. Starting with the question of the purity of the substrate, quality of the HI (but
this sounded ok, 4 hours should have been enough though), to the point of the missing step of drying the toluene before gassing with HCl.
For I always think the best of people I believe that the member didn´t really break a law. At least not more then the people who are making TNT here.
regards
/ORG
PS: Hey! You didn´t basify the post reaction mixture, how do you think to extract what you want? You must add LYE and not water and then SEVERAL
portions of toluene, and mix the stuff decently, damn it!
Your extract shouldn´t be red.
Now you know where your stuff is. Basify, extract, gas, identify and destroy. Thats the usual way this is done. Destruction of explosives is usually
done by controlled explosion. Your stuff can be destroyed by bleach or biological degradation.
[Edited on 23-7-2006 by Organikum]
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Nicodem
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But Organikum, how can you be so sure he was not trying to synthesize iodine by oxidation of HI with ephedrine? After all he seams to be after the
reddish stuff:
"...after a good swirl, the reddish seemed to go in the toluene, the aqueous bottom layer seemed to clear up..."
In such case I believe he almost did well to remove the byproducts by extraction of the acidified solution with toluene. If he would basify it first,
then the extract might get contaminated by the reaction side product which is a base. Furthermore, the iodine disproportionates to iodide and
hypoiodite with the addition of lye. So I2 could not be extracted. I however have no idea where he heard that I2 can be precipitated from toluene by
gassing with HCl. He must have made confusion with some other procedure. I also don’t know how he is going to isolate I2 from toluene in any simple
way. It would have been much more advisable to use CH2Cl2 to do the extraction as it has a low enough b.p. to allow for evaporation from I2, though
with great loss due to sublimation.
All in all, I have to admit this is a very ingenious way to oxidize tediously self made HI to I2 and a viable way for its preparation. Provided that
you destroy the side products, of course. Biodegradation? Yeah sure, that should do. But check the local law anyway.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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chemoleo
Biochemicus Energeticus
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Sorry for asking this almost newbish thing... I am not really into all this 
From what I understand, the starting compound P.E.
is to be converted to one where the OH is replaced by H.
With HI, it would form the I-R. The question is, what is the mechanism of conversion to H-R. I understand why NaOH etc is required (to make the free
amine, which dissolves in toluene), but noone actually commented on this required conversion.
[Edited on 25-7-2006 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Organikum
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R-OH + HI = R-I + H2O
R-I + HI = R-H + I2
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DDTea
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| Quote: | Originally posted by Organikum
R-OH + HI = R-I + H2O
R-I + HI = R-H + I2 |
If water is formed in the first step, adding silica or some other desiccant should help the reaction along.
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Organikum
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H3PO4 or GAA are the means of choice to keep the concentration of the HI up. I would recommend H3PO4. The reaction proceeds as long as the
concentration of the HI is >45%. Of course one can just add red phosphorus ....
[Edited on 24-7-2006 by Organikum]
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garage chemist
chemical wizard
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What about adding gaseous H2S? It reacts with iodine, forming sulfur and HI.
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Organikum
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H2S and iodine form HI only up to a concentration of 35% or so says Herr Erlenmeyer, HI produced from H2S and I must be redistilled to be useful for
such reductions.
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chemoleo
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Why this choice of H3PO4, or GAA? Why not just H2SO4?
Also, what's the reaction then between rP and I2? PI3/PI5, which then hydrolyses with H2O to form HI?
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Organikum
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H2SO4 if not very diluted oxidizes HI. The choice of H3PO4 over GAA is mainly that it doesn´t stink so badly. HCl could be used as a cosolvent but
this requirers then a pressurized setup.
3I + P = PI3
PI3 + 3H2O = 3HI + H3PO3
The H3PO3 itself reacts again with iodine and water:
2I + 2H3PO3 + H2O = 2HI + 2H3PO4
On a sidenote:
The PI3 formed in the first step also is able to iodinate the alcohol directly IIRC
[Edited on 24-7-2006 by Organikum]
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hodges
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Don't forget to add some water or something to slow the reaction down. My apologies if this link has been posted here before. I thought it was
pretty funny. This guy may even be eligible for a Darwin award, considering one of the parts of his body that was burned 
<a href=http://www.foxnews.com/story/0,2933,127839,00.html>link</a>
Hodges
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len
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cyberzed. I do hope you posted and registered from the uni library or something because the internet only appears anonymous. and Im sure this forum
is watched
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DeAdFX
Hazard to Others
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[paranoia]Or it could be one of the watchers trying to see if we are drug forum[/paranoia]
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Nicodem
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I don't think anybody gives a f**ck about somebody trying to do a 1g batch. Especially since without having the basic knowledge of what he is doing
would most likely take care of the punishment by himself in form of injuries or burns. The fuss of tracking down internet communications would
certainly not be in proportion to the (non)severity of such law breaking.
My reply to Cyberzed was only to scare the guy as it was obvious from his post that he did not really take enough care to learn basic chemistry before
starting. It was not to provoke paranoia.
Paranoia is completely out of place here, at least unless you live in the US or unless if it is stimulants induced paranoia (which is actually the
same thing).
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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Organikum
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This paranoia is nonsense, the discussion of chemistry is still legal.
Here at SCM you can discuss everything science and in special chemistry related, the only restrictions are:
- use of scientific language and not druggie/cook/kewl speech.
- pictures and movies of the detonation of explosives are only permitted if the compound is new or employed in a new and sophisticated way.
- if insensitive questions are asked which are aimed to the preparation of problematic compounds one better has gathered some serious knowledge and
present it or you most probably go to Detritus.
- you have to use proper capitalisation
/ORG
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Organikum
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But back to the really rather interesting question of the reduction of alcohols by HI and ways to do this.
I read once an old german article where they employed 95% H3PO4 as solvent and used NaI or KI instead of iodine with a rather small amount of red
phosphorus to recycle the formed I to HI again.
Thats an elegant solution:
- it calls only for NaI/KI whats much easier to get and not so nasty as pure I.
- the H3PO4 dehydrates the reaction and ensures an always very high concentration of free HI in the reaction.
- the H3PO4 mediates the heat formed in the reaction
Using H3PO2 or H3PO3 instead of the P would be even better.
/ORG
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Filemon
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| Quote: | Originally posted by Organikum
H2SO4 if not very diluted oxidizes HI.
[Edited on 24-7-2006 by Organikum] |
I have used H2SO4 to make HI, I have not seen crystals of I2.
How much time takes the reaction of oxidation at ambient temperature?
H2SO4 + HI ---> H2S + I2 + H2O
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Organikum
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Care to elaborate how concentrated the H2SO4 was and what concentration of HI resulting was?
All literature states that this is no feasible way to produce HI of a useful concentration + the question of separation.
And it is:
H2SO4 + HI = SO2 + I + 2H2O, the Bunsen reaction.
This reaction is reversible depending on concentration of HI and H2SO4.
Also this page claims that HI is in the laboratory produced from conc. H2SO4 and NaI I say thats plain bullshit and every better chemistry textbook
says the same. I suppose it´s knowingly misleading information related to WoD.
[Edited on 25-7-2006 by Organikum]
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len
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Organicum, what you want and what the law allows are quite different. Not capitalising wont get you time in jail, but making drugs will. There is no
fuss in "tracking internet communications", I can see where people visiting my site are and where they have been. Sometimes I can tell both the
company and the city. And Im not the police. Would you rather engage in chasing dangerous criminals through the streets, or tracking net traffic in
a warm office? Plus Im sure site management has presented this as a good reason to be allowed to keep the forum, that way things are under control.
You have to strike a balance between paranoia and naivity.As far as the reaction goes its a piece of chemisty trivia, given the basic structure is
already there, of interest only to drug makers who want the simplest route possible.
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Organikum
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Then chemoleo who asked for some information about this reaction is a "drug makers who wants the simplest route possible"? Interesting.
Anyways, it´s not your board and not mine, but Polverones. The topic whats allowed was discussed before and I just repeated the outcome. Take it or
leave it.
And whats this board about? To a very big part it´s about the discussion of ways to produce compounds one wants by the simplest way available to
amateurs.
/ORG
[Edited on 25-7-2006 by Organikum]
[Edited on 25-7-2006 by Organikum]
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Nicodem
Super Moderator
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| Quote: | | Not capitalising wont get you time in jail, but making drugs will. |
That is simply not true. Only few drugs can get you in jail. Many of the best drugs are completely legal in most countries. One should always check
the regulations before planning the synthesis of a psychoactive compound and if the compound is scheduled, rather make a legal analog instead. That's
where literature search skills and knowledge on structure-activity relationships comes handy.
And I do believe that not capitalizing can get you in jail, though indirectly. It shows ones’ illiteracy, which leads to stupidity and stupidity is
one of the main factors on why people end in jail.
| Quote: | There is no fuss in "tracking internet communications", I can see where people visiting my site are and where they have been. Sometimes I can tell
both the company and the city.
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Well, except for a couple of countries with totalitarian tendencies, the police needs a warrant in most others to get such information from the site
manager. That's why I said that there is no need for paranoia except if you live in US. Sorry if I forgot Australia, but I'm not familiar with what's
going on down under. Surely there are other such countries where freedom is not valued, but only the minority of the world population has the
misfortune to live there.
I trust Polverone to not worry if he can access my IP loggings and I trust that he has chosen a trustworthy server provider. And even if he did not,
why should I care. Neither do I do any noteworthy illegal activities neither do I live in the country where the server is located. As far as for such
fools that send confessions on the board, they are responsible for themselves. It is not the responsibility of the administrators or members to keep
them out of troubles.
| Quote: | As far as the reaction goes its a piece of chemisty trivia, given the basic structure is already there, of interest only to drug makers who want the
simplest route possible.
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The HI mediated reduction of alcohols is anything but trivia and is mechanistically a very interesting reaction. I find it very fascinating even
though I'm not a "drug maker" making meth from ephedrine. And I'm sure Chemoleo is not the only non "drug maker" interested in the underlying
mechanism of this reaction. So Organikum's explanations and commentary is quite probably interesting to some other members as well.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
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len
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Look, you both misunderstood me. I was not attacking Organikum. I dont think chemoleo is a drug maker (judging by his postings, I dont know him) and
its not for me to judge his cursory interest in the reaction. But cyberzed certainly is a maker. I note he only posted once and then waited for the
returns (watching as guest of course). If he was just interested in the hydrogenation of alcohols he might have chosen a less dangerous example.
The point is this forum is acquiring people from a recently closed down forum. And might just follow it. Do you want that.
I dont see the challange in this reaction. A carpenter was recently busted for doing it, it was in the papers, which shows you dont need to know any
chemistry for it. That is why most makers prefer it. Its only consequence for me is that iodine and iodides can only be purchased with a lot of
paperwork. Thanks cyberzed!
[Edited on 26-7-2006 by len]
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Organikum
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Hey len, may I suggest that you just look around a little bit here on this board and make yourself comfortable so know the conventions before you
start to tell members what they have to do, what they have to post and what not etc?
You may discover for example that here we talk absolutely open about sources of chemicals. Duh! Horrifying I know but we do. Since years.
Also I have all respect of carpenters. I should, as I learned this craftmanship before I went to the university. This experience makes me believe that
a lot of the good old chemistry is better done by a craftsman then by one of these Sigma-Aldrich addicts.
Finally I want to ask you a question len: Do you by accident take amphetamines? Prescribed ones or others? You sound to me a little bit like a acute
case of speed paranoia. I should know this. I was on speed for years, but then I layed off the habit with the help of a lot of LSD. But to be true, I
don´t think I was ever so paranoid as you are now although I knew quite some methheads who beat you still. Talking to the shadowpeople and such.
So what I wanted to say is: Relax.
regards
/ORG
PS: I don´t do drugs any more except a joint occasionally whats more or less legal here where I live.
[Edited on 26-7-2006 by Organikum]
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