| Author |
Topic:
Hex>>>>to>>>>>amine--Results |
Sumerian Member |
posted 06-02-99 10:25 PM
Needed some amine so this is what I did in 8 hours total time.I had posted
this procedure awhile back,and thought I'd post again for those who missed
it.Anyhow took 80g Safesport hexamine camping fuel,added 300ml 28%Hcl,and
set-up vaccum reflux.Refluxed mix at 65c for 4 1/2 hrs with good magnetic
stirring.Then rigged for vaccum distillation and distilled off liquids til
flask was full of crystals ~75c was peak temp during distillation.Took
flask of crystals and added ~150ml acetone and vaccum filtered the
crystals.Took filter cakes and weighed at ~150g.Put crystals in beaker
added ~100ml chloroform(I know I didnt need to do this,but I wanted to
prove a point to myself)swirled well and vaccum filtered
again,reweighed,no loss of weight.This time I didnt do the alcohol
extraction bit because I know that the temp stayed low enough to avoid any
by products,so I went straight to acetone clean-up.This method is by far
better than any other I have done to date,but there was a special surprise
this time>>>no ammonium chloride formation,I tell you that there
was none anywhere to be found.This is a quantitive yield I suppose.I
evaporated all cleaning solvents used and there was no residues or
"by-products".Everybody I plead to you,try it this way,you'll never look
back.Temp is the whole key,use the water bath! Others reflux temp may vary
with vac capabilities,my vac only pulls 23 Hg.
Regards,Sumerian
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sunlight Member |
posted 06-03-99 10:55 AM
Why do you know there's no ammonium chloride ?
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Semtex
Enigma Member |
posted 06-03-99 12:02 PM
I have to agree with our Sunny friend, there is nothing that you've said
that would take out or hinder the formation of the ammonium
chloride...
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Sumerian Member |
posted 06-03-99 01:48 PM
Well the end product shows it all,sorry I cant convince you otherwise.I do
know the purity of my final product.I evaporated all solvent "washes",they
all evaporated with no residue,if ammonium chloride was dissolved in any
of the washes,it surely would reappear upon evaporation.Can any of your
peoples methods produce 150g methylamine from 80g hexamine? A close friend
has analyzed my "product" in his work lab,99.9% believe it or not.I'm not
posting this stuff to gain anything,its here for all of you.I dont
bullshit around like others Ive seen here.Dont believe it if you dont want
to,go ahead with longer less yielding methods.I have some other info that
could change some things dramatically here,but I see it would be too much
of a hassle for anyone to accept.So on that note this will be my last post
here on the hive. Its been real,Regards Sumerian
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Penis
Seinfeld Member
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posted 06-03-99 02:14 PM
I don't understand. Why are you getting all worked up, Sumerian? They were
merely asking for proof. You expect everyone to accept your procedure at
face value? Please, not even the Rev. Drone gets such special treatment.
They asked you a simple question, they didn't attack you.
PS
|
Semtex
Enigma Member |
posted 06-03-99 07:30 PM
Sum, i'm not flaming you, I personally have a VERY limited knowledge of
chem. I was under the impression that Hex was or formed a mix of
Methylamine and ammonium chloride, sorry if I sounded like a prick, that
was not my intention...
|
Jabber Member |
posted 06-03-99 09:36 PM
Excuse my ignorance, but how does one setup for vacuum reflux? Is the
vacuum source attached to the top of the condenser, or is a vac adapter
with an empty flask put on top?
- Jabber
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Shlong Member |
posted 06-03-99 11:46 PM
Sumerian, I really do appreciate your posted method even though I havn't
commented on it previously, and I do believe you !! I will dream your
method and report back to the hive to back you up and give you the true
credit you diserve on this reaction, provided it works, which I'm sure it
will. It just takes a little time to secretly set up my lab.
|
equarius Member |
posted 06-04-99 01:16 AM
If this works as it sounds like it does then a major advance in amine
production has been made. The amount of labour is completely minimized.
I am a bit sceptical of the 150g MeAmineHCl from 80g Hexamine when a
regular hex to Mex might yield 40-60% by weight. How is this possible? The
calculations are beyond me. Why not work it up regularly just to be
sure. Ie an alcohol recrystallization, then a chloroform wash to remove
any excess Hexamine.
Jabber; let me know if I can help in confirming his results. I think a
vac reflux setup could be done with a conventional distil kit by
assembling a single neck flask, then condenser, then vac adapter at the
top with the big hole sealed and vac on the vac port.
Sumerian; Dude please don't leave. Your work is inspirring, someone
will try to confirm it soon. It's just that people are naturally sceptical
around here with stuff like the PdAcetate fiasco, the MDP-pol fiasco, etc
etc. I would eagerly attempt to confirm your results but am labless for
the time being. I hope you'll continue to make more groud breaking
contributions.
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equarius Member |
posted 06-04-99 02:10 AM
Please elaborate of what exactly you mean by reflux. As in the correct
term of boiling, or as in heavy CO2 evolution?
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sunlight Member |
posted 06-04-99 02:56 AM
Sumerian, forget all the misunderstandings, My idea is that we are a
fantastic whole reasearcher group. Nothing personal or something like
that. Any invention of a bee will benefit all the comunity. What I want
to mean is that it's possible you have an error in the design of your
procedure, and then you have wrong results. When is removed the ammonium
chloride ? In the washes ? So you believe that amonium chloride is solble
in acetone or chloroforme, but methylamine chloride is not. I doubt
it. If you remember I encoureged you to determine the melting point of
your product last time, and your data was very satisfactory, but if we
want to get pure chemicals we need refined procedures of purification.
Acetone will dissolve hexamine, and chloroforme dimethylamine HCl, but
if ammonium chloride it's present, like in the regular procedure, I don't
see any point where you remove it. This is a dark corner. Now we have a
new info, you say your product has been analyzed and it is 99.9 % pure, so
it seems that this rxn doesn't produce byproducts. It would be fantastic,
certainly. I hope some other bee can confirm your research. With no
purification it could be converted in methylamine in meethanol for the
high yielding and ecological LabTop's NaBH4 procedure. And don't bother
with a bit of scepticism, we need it, we have seen "great inventions" that
were finally nothing.
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Shlong Member |
posted 06-04-99 07:34 AM
Dear Reverend Sumerian, was that 23 mm or inches that you vac pump pulls.
This is important to help me back up your new breakthrough. Thanks.
/Sg.
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prickleberry Member |
posted 10-04-1999 09:49 AM
Had a day dream about doing this method and crude yield was around the
50%. After cleanup it was much less. Prickleberry was not impressed !!
Prickleberry
thinks damn you Sumerian !! Hope you got your jollies posting this bogus
overated + over inflated yields method.
Can anyone back up our friend Sumerian or is he on his own ?? He must
have made a major boo-boo somewhere in his observation. Maybe 95% yield =
MeAmCl + AmCl . If so, I did get 95% yield !!! WOW, I feel much better now
......Any comments or flames to add......feel free !!
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FMAN Member |
posted 10-04-1999 06:13 PM
Shlong it Torr unless otherwise stated ussually. It was very clear to me?
I belive the starting product could be the difference, did ya all use
the name brand?
Lastly the Sumerian never did exactly state the final product allthogh
I think it is methylamine fr4om
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FMAN Member |
posted 10-04-1999 06:17 PM
the post makes no reference explictly to other tests preformed or the
specific type of test it could be the only test was for the paticuliar
ammonia compound, the thing looks good as is to me??
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ChemHack Member |
posted 10-14-1999 11:14 AM
Ammonium Chloride almost insoluable in dry Acetone. Try it yourself.
Summerian's write up does not account for possible ammonium chloride
contanimantion, which you would expect to be the major side product
weighing 50% or more of the total product's weight.
A mixture of ammonium chloride and MeAm.HCl will be very hard to
distinguish from a pile of pure MeAm.HCl because ammonium chloride has no
significant odor. The mixture will melt in air just as pure MeAm.HCl will
so that is not a reliable test either. Also, a chemical test that only
tests for an amine will show true for both products.
Finally, ammonium chloride would not interfer with Al/Hg amination
procedures. The ammonium chloride, even though it is less reactive, will
still form MDA. Most people won't complain about MDMA that has been
contaminated with MDA This amination
procedure calls for a molar excess of MeAm.HCl so using a contaminated
product may even result in no loss of total yield of MDMA.
The possibility that ammonium chloride could have easily passed through
Sumerian's purification process does not mean that it did infact pass
through. An easy way to detect ammonium chloride would have been to
attempt to dissolve the product in dry boiling alcohol.
It is my assumption that Sumerian's product was far from quantitative
and actually contained quite a bit of ammonium chloride. I have not
duplicated the proceedure so this is only speculation on my
part.
|
Mephistopheles Junior Member |
posted 10-14-1999 11:57 PM
The good doctor Faust has done this reaction for me several times. As long
as he keeps the reaction temperature low, methylamine is the predominant
product of the reaction. There seems to be a relationship between the
temperature and the amount of ammonium chloride found in the final
product. If the temperature gets over 110C almost no methylamine is
formed.
Dr. Faust informs me that using an aspirator has several benefits. That
nasty smell is sucked down the drain and covered up. In fact, placing a
bubbler filled with an H2SO4 solution between the receiving flask and the
aspirator make the smell almost nonexistant. Also the entire process of
removing the water goes much faster, more methylamine is produced, and
less ammonium chloride is present in the final mixture.
If I have time, I will instruct one of my underlings to research the
kinetics of this reaction and use his knowledge of physical chemistry to
derive the "optimum" temperature for this reaction.
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hellman Member |
posted 10-17-1999 10:02 PM
Yes,
I have not ran this same scenerio several times, different reflux
temps, longer periods, different brands of hex, etc,. and have found very
different results,.
I can't put my chemistry challenged finger on it, but almost every time
i ran this experiment, the hexamine would dissolve into the HCl, then
while being left over night, no reflux- 24 hour wait at 20C, these
crystals would appea, depending on reflux temp, the warmer the reflux the
yellower/greener the crystals would become, Although at the time being
an idiot, i noticed that the first crystals (pure whitethat form in the
wet HCL solution were almost mousse like in texture, or even gelati
like,. I assumed this shit to be the contaminant, which I filtered off,
to leave me with this greeny solution, which hence dried to give me what i
thought to be methyhlamine,.
gotta go
hellman
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hellman Member |
posted 10-17-1999 10:07 PM
So all I am trying to say is that, there can be alot of variations in
final product with this method,depending on conditions. Personally I do
not trust this method, as I cannot see it backed up in any
literature,. Although If it is working in the final animation for some
bees, then so beeee it. Personally i am and always will be the
acetamide man, it's just much more otc down here,.
hellman,
If it's true and and can be tlc, nmr tested, then You have done well!.
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