Author Topic: For the vindication of Eleusis - Methylamine  (Read 56785 times)

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armageddon

  • Guest
oh no - not again
« Reply #80 on: July 21, 2004, 07:32:00 AM »

abolt

  • Guest
You sure do seem to contradict yourself a lot.
« Reply #81 on: July 21, 2004, 12:00:00 PM »
You sure do seem to contradict yourself a lot. First you say:

I DID NOT STATE THAT ANY DISTILLATION HAS TO BE DONE SLOWLY TO GET GOOD RESULTS WITH SAID IG_FARBEN PATENT!!!

.....and then you say:

THE CAREFUL DISTILLATION IS BTW NEEDED IN ORDER TO AVOID DISTILLING AWAY SOME ETHANOL BEFORE ALL EXCESS FORMIC HAS HAD ENOUGH TIME TO REACT WITH IT!

DID YOU REALLY MEAN YOUR SUGGESTION AS A SERIOUS RESPONSE TO MY LAST POST??

I think you are an "armchair expert" and a plagiarist.

I tried it, and if temperature is controlled in the way described above, it is possible to collect ALL of the theoretical amount of ethylformate in a temp. range BELOW 43°C

Brilliant.........you manage to distill Ethyl Formate below it's Boiling Point of 54 Celcius.

http://ptcl.chem.ox.ac.uk/MSDS/ET/ethyl_formate.html




abacus

  • Guest
I agree abolt
« Reply #82 on: July 21, 2004, 12:48:00 PM »
arm chair expert, I mean "arm chair useless", is full of words such as.

"I think, I would believe, maybe you, i suggest, might be, I wouldn't advise" etc etc ...it doesn't convince me armegeddon has actually tried this synth.

This thread is supposed to teach us new and improved ways of increasing our yields from bees that have actually gotten home from school and tried to make some shit, useless debate from armchair experts isnt making it any easier.

But the challenge has been made, so experimental reports on the effect of adding ethanol to this procedure will soon follow.

Abacus

armageddon

  • Guest
useless for morons...
« Reply #83 on: July 21, 2004, 05:12:00 PM »

abacus

  • Guest
QED
« Reply #84 on: July 22, 2004, 12:16:00 PM »

Bond_DoubleBond

  • Guest
swim has had great success with refluxing,...
« Reply #85 on: July 23, 2004, 01:48:00 AM »
swim has had great success with refluxing, distilling off the formate quickly, then allowing the reaction to proceed at ~100c. 

slow heating and distillation is NOT necessary.

abolt

  • Guest
slow heating and distillation is NOT ...
« Reply #86 on: July 23, 2004, 05:12:00 AM »

moo

  • Guest
Sheesh.... grow up.
« Reply #87 on: July 23, 2004, 06:18:00 AM »

armageddon

  • Guest
oh - how pissed of I am now!!
« Reply #88 on: July 23, 2004, 07:35:00 AM »
swim has had great success with refluxing, distilling off the formate quickly, then allowing the reaction to proceed at ~100c. 

slow heating and distillation is NOT necessary.


Not necessary for what - for just making methylamine? Noone said so....

You can even reflux just hexamine, NH4Cl and HCl and hold at 105°C and get good yields, and nobody wants to keep you from doing so (at least if you are the only person working in your lab - cough, cough..)

Did you use a column? At which temp. came the ethylformate over? And (most important to me) did you get any diMeAm, what about formaldehyde stink - was there any? Most important: how was the yield?

All in all, your statement is of no more reliability than mine - how about sharing some details? It seems you don't consider it necessary to properly separate the EtCOOH from unreacted EtOH? Could you please tell us if/why/how you came to that conclusion/observation/whatever?

Abolt, it appears that you should consider yourself lucky that I don't know you personally. Don't want to lose any more words about credibility, besides of this: In no way will I get A NEW USERNAME just because some debile dumbass screams "You were wrong, you were wrong" when some other bee writes he has had success with some slightly different procedure. And most surely I won't do so just because ABOLT is the one to scream.. (abolt, do you often change your user name when you fear about your credibility??? coward..)

(everybody else - make your own opinion about credibility of my posts)

I sadly fail to understand Abolts motivation: do you want to convince all readers of this thread to use the standard NH4Cl/HCHO method? Or do you believe the method is just bogus and doesn't work better than any other one??

If that's the case: ABOLT, MAY I SUGGEST YOU MAKE YOUR OWN THREAD THEN??????????

Greetz A


armageddon

  • Guest
reliable or not - my thoughts...
« Reply #89 on: July 23, 2004, 08:12:00 AM »

Organikum

  • Guest
The method like outlined by BDB works well...
« Reply #90 on: July 23, 2004, 10:52:00 AM »
The method like outlined by BDB works well after my experience, it is for sure the FASTEST way to make methylamine from hexamine in yields which dont stand back to those yielded with the old timeconsuming method.

The other ways discussed by armageddon and amalgum are not as fast but promise better yields. It are optimisations on yields.

There is no contradiction.

I want to thank all who post practical experiences here - there is more than one way to skin a cat, lets discuss it  ;D . Its always good to have choices, some with better equipment and more time will prefer a slower but higher yielding method, the method as told by BDB is a present to all whos time is pressing.

Nevertheless I am astonished what kind of behaviour of a certain immature member is tolerated here - I thought this forum is moderated.

thanks
ORG


abolt

  • Guest
The "optimised" BDB/abacus version
« Reply #91 on: July 23, 2004, 10:55:00 AM »
armageddon & organikum

You have both taught me a valuable lesson, and that is that a bee that is prepared to roll up his/her sleeves, put some glassware together, and do some actual research is worth more than all the bullshitting "armchair experts" on the planet.

Nevertheless I am astonished what kind of behaviour of a certain immature member is tolerated here - I thought this forum is moderated.

Do you think that the reason that I have not been, as you say, "moderated", is that I may have a point?

I am quite happy for the members to go back over this thread and make up there own minds as to who has been productive and counter productive.

Let's agree to not pollute this thread with any more of your stupidity.

To save yourselves any further public embarressment, you can P.M. your apologies to me.

Now, here is some more USEFUL information.

After reading the interesting words of abacus:

Setup for redistillation and distil again at atmospheric pressure UNTIL the flask contents temperature is OVER 150DegC, Then pour into a container and cool.  This will cause the whole solution to form a solid. 


in his (EDIT - THE WORD THREAD HAS BEEN REPLACED WITH THE WORD POST, APOLOGIES FOR THIS OVERSIGHT, ALTHOUGH I ASSUME THAT MOST OF YOU WOULD HAVE BEEN INTELLIGENT ENOUGH TO WORK THIS OUT ANYWAY :) ) post:

Post 513530

(abacus: "Alcohol is not vital", Methods Discourse)


abacus, then goes on to say:

This seems like a lot of crystallising methylamine.hcl but its not.

Maybe so abacus my friend, but if you substitute the first part of the I.G.Farben patent as mentioned by BDB:

Post 500578

(Bond_DoubleBond: "Nothin special, but here ya go . . .", Methods Discourse)


for the Vogel procedure you are left with a MeNH3Cl that is suitable for the Osmium Al/Hg. ;)

Swim set about to do another experiment, using some of abacus's interesting workup.

After formate distillation, excess NH4CL removal and the 1 hour reflux, glassware was set up for distillation and the oilbath was raised to 155 Celcius (as measured by a thermometer dipping into the reaction) and held there until water distillation ceased. The distilling flask was quickly removed and the contents poured into a beaker whilst still hot.

The beaker was left to cool to room temperature and formed a hard white sheet of solids, that was crushed up and vacuumed filtered to allow for around 10 mls of liquid that was crashed out with dry acetone to give a very small amount of MeNH3Cl. The resulting dry crystals in the buchner was thoroughly rinsed again with dry acetone and vacuum filtered again and gave no appreciable weight loss. Tests done on the crystals showed them to be at least 93% weight MeNH3Cl.

This research is also in accordance with the yields noted by BDB (92% & 94%):

Post 512674

(Bond_DoubleBond: "not to worry . . .", Methods Discourse)


My point is that MeNH3Cl for a standard 3 x excess Osmium Al/Hg, can be made without recrystallisation, the use if vacuum or vacuum filtering and with "ghetto" equipment if need be.

I know this might offend some of the purists out there, but please consider:

Simply add the required amount of reactants, quickly distill off the formate, reflux, filter, distill and hold reaction temp at 155 C until H2O distillation ceases, quickly pour out, let cool, crush up solids and add aqueous 25% naoh until neutral.

Easy as pie :)  

This is just bits and pieces of other peoples techniques.


Thank god for research. ;)


Organikum

  • Guest
You are telling me to stay out of my own ...
« Reply #92 on: July 23, 2004, 11:42:00 AM »

armageddon

  • Guest
finally something worth reading!!!!
« Reply #93 on: July 23, 2004, 11:45:00 AM »
Thanks abolt - I was starting to think you REALLY were an armchair expert, now I know better.

But, sorry to question you again, and this is ABSOLUTELY NOT meant as an accuse/flame or anything negative:

The only difference between yours and mine procedure, as far as I can see, is the time needed for formate distillation (you: quick - me: slow) and the workup (you: dirty - me: clean)...

Your 1h reflux is essentially the same as my normal H2O dist./removal at ambient pressure WITHOUT refluxing before - the temp. at least is exactly the same, whether refluxing or distilling water. So maybe it isn't even necessary to perform the one hour extra reflux.

How do you be sure about the crystalline solids being 92%+ MeAm*HCl? Any test/analysis? And how then? (only interest, not disbelief)




And another thing that looks a bit strange in my eyes..

You say:

"Swim set about to do another experiment, using some of abacus's interesting workup.

After formate distillation, excess NH4CL removal and the 1 hour reflux, glassware was set up for distillation and the oilbath was raised to 155 Celcius (as measured by a thermometer dipping into the reaction) and held there until water distillation ceased. The distilling flask was quickly removed and the contents poured into a beaker whilst still hot.
"

Where is "abacus' interesting workup"? Is it the pouring of the concentrated solution, the vacuum filtering or the acetone rinse? (not to offend you abacus) I mean, none of these results in separation of side- and main products (DiMeAm, MeAm and AmCl) AFAICS.

And the temperature of heating baths is measured by placing a thermometer below the surface of the heating liquid - with measuring inside the flask, it is called "reaction tempearature", not oil bath temperature...

Oh BTW you really don't have to strictly refrain from referring to other bees posts - BDB is not the only one having had success with it, and Orgy did "discover" the patent for the hive, translated it and tested its workability before posting about it - do you really think you can tell him what to do and not in this HIS OWN thead, while discussing YOUR variation of said patent inside this thread? Again, this is IN NO WAY meant as an accuse: maybe you should just open a new thread, called "Easy Ghetto Methylamine in +90% yield" or something like that maybe - I'm sure it would be read by *lots* of bees.

But really, you wouldn't know about ANY pros/cons of ethanol addition to hex/HCl if Organikum wasn't here... Ask yourself the question: is it right to flame him (me = OK  ;D ) - just because he did so with you? Remember that you first questioned what you now seem to accept as a fact (ethanol=good). And I can understand quite well why Org. flamed you for not believing him in the beginning...

(my personal apologies - for being that hard with you...  ;D )

A


abolt

  • Guest
How do you be sure about the crystalline ...
« Reply #94 on: July 23, 2004, 11:59:00 AM »

armageddon

  • Guest
faker!
« Reply #95 on: July 23, 2004, 12:00:00 PM »

hypo

  • Guest
like who cares?
« Reply #96 on: July 23, 2004, 12:13:00 PM »

abolt

  • Guest
^^^^^Nervous breakdown in progress^^^^^
« Reply #97 on: July 23, 2004, 12:14:00 PM »

armageddon

  • Guest
better not
« Reply #98 on: July 23, 2004, 12:37:00 PM »
I recommend you try to overead each of his nonsense posts - especially the one where he claims a 93% (and more!!) yield/purity of MeAm, although it is obvious that some ammonium chloride will stay in solution even after removal by fractional crystallization.

It is ABSOLUTELY pure bullshit to claim the YIELD being 93 percent - without making sure that the product in question is really what you made/isolated!

Just cooling between reflux and concentrating precipitates by far not all ammonium chloride - a healthy amount will stay in solution UNLESS you use a technique based on different solubilities COMBINED with drying the solid salts to be separated BEFORE attempting this technique - which is commonly called "soxhlet" or solid/liquid extraction - useful solvents are alcohols in this case, the higher the better...

(I don't care if abolt is stupid as bread or not, I justz want to prevent others from getting disappointed)

A


abolt

  • Guest
POST No.100
« Reply #99 on: July 23, 2004, 12:49:00 PM »