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Author Topic:   Hex>>>>to>>>>>amine--Results
Sumerian
Member
posted 06-02-99 10:25 PM     Click Here to See the Profile for Sumerian     
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

sunlight
Member
posted 06-03-99 10:55 AM     Click Here to See the Profile for sunlight     
Why do you know there's no ammonium chloride ?

Semtex Enigma
Member
posted 06-03-99 12:02 PM     Click Here to See the Profile for Semtex Enigma     
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...

Sumerian
Member
posted 06-03-99 01:48 PM     Click Here to See the Profile for Sumerian     
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

Penis Seinfeld
Member
posted 06-03-99 02:14 PM     Click Here to See the Profile for Penis Seinfeld     
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     Click Here to See the Profile for Semtex Enigma     
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     Click Here to See the Profile for Jabber     
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

Shlong
Member
posted 06-03-99 11:46 PM     Click Here to See the Profile for Shlong     
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     Click Here to See the Profile for equarius     
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.

equarius
Member
posted 06-04-99 02:10 AM     Click Here to See the Profile for equarius     
Please elaborate of what exactly you mean by reflux. As in the correct term of boiling, or as in heavy CO2 evolution?

sunlight
Member
posted 06-04-99 02:56 AM     Click Here to See the Profile for sunlight     
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.

Shlong
Member
posted 06-04-99 07:34 AM     Click Here to See the Profile for Shlong     
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.

prickleberry
Member
posted 10-04-1999 09:49 AM     Click Here to See the Profile for prickleberry     
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 !!

FMAN
Member
posted 10-04-1999 06:13 PM     Click Here to See the Profile for FMAN     
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

FMAN
Member
posted 10-04-1999 06:17 PM     Click Here to See the Profile for FMAN     
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??

ChemHack
Member
posted 10-14-1999 11:14 AM     Click Here to See the Profile for ChemHack     
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     Click Here to See the Profile for Mephistopheles     
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.

hellman
Member
posted 10-17-1999 10:02 PM     Click Here to See the Profile for hellman     
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

hellman
Member
posted 10-17-1999 10:07 PM     Click Here to See the Profile for hellman     
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!.

All times are CT (US)

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