02-15-04 13:12
No 488907
Swim just got done with swims first attempt to make methylamine HCL from Hexamnine. swim used Eleusis's method with comments from Rhodium. But swim is little confused. After adding hexamine to the acid/alcohol swim didnt get a lot of fuming as it seems to portray in the reciepe. In fact it didnt really fume or smell except a little bit. So swim capped and stirred the solution magnetically for 18hrs and it did get cloudy as through a precip was forming. But when swim put the solution thru the Buchner funnel the whole soltion went thru the filter paper and into to flask. No white precip. had formed. All swim had in the funnel was wet filter paper. Confused at this point swim pressed on. Swim heated the solution and concentrated it. Swim did notice toward the end of concentrating the solution it began to form a skin on top of it like milk does when you heat it. Anyway Swim turned the heat off shortly after that and as the solution cooled it soldified more and more until Swim had a pyrex dish full of semi soild white crystals(still wet, Swim guesses). So swim scraped them into a sep funnel and added the methanol, shook the hell out of it and let it sit. Swim notied two layer form. On bottom there are the white crystal solids, on the top there is a tannish yellow semi clear solution. And thats exactly where swim is right now. Shits sitting in the sep funnel right now. So whats the crystaline stuff on the bottom is it Methylamine HCL or is it Ammonium Cholride. Does swim need to evaporated the top layer to get the methylamine or what. I'm confused. Please Help
When the going gets wierd, the wierd turn Pro. HST
(Hive Addict)
02-15-04 21:41
No 488969
So whats the crystaline stuff on the bottom is it Methylamine HCL or is it Ammonium Cholride.
Most likely Ammonium Chloride.
Does swim need to evaporated the top layer to get the methylamine or what. I'm confused.
Filter the lower crystals and place them aside. take the Meoh mixture and place it in a beaker in the freezer. Methylamine flakes should precipitate.
You have chosen a peculiar and innefficient way to make Methylamine. Choose another way and read more up on the subject.
.......or you could try this
What you will need (scale to suit your needs)
1 x 3 litre 3 neck flask
1 x 2 litre R.B.F.
1 x 1 litre R.B.F.
1 x still head
1 x condenser
1 x vacuum adaptor
1 x thermometer (a good quality one with single degree measurements)
1 x hotplate stirrer
1 x egg shaped stir bar
1 x Buchner funnel
1 x vacuum flask
1 x beaker (or suitable alternative)
1 x vacuum source (aspirator is sufficient)
vari0us stoppers
560 grams Hexamine(4 moles)
1950 mls of 30% Hydrochloric acid (16 moles)
400 mls DH2O
1. In a 3 litre 3 neck flask, set up for standard distillation in an oil bath, upon a hotplate/stirrer, was placed 560 grams of crushed Hexamine, 1950 mls 30% HCl and 400 mls DH2O, with the 2 litre R.B.F. as the recieving flask.
2. In One of the side necks was placed a thermometer that was immersed well into the mixture and the other side neck was sealed up. The still head was also sealed with a stopper.
3. The hotplate stirrer was turned on and stirring and heating was commenced.
4. The temperature was closely watched on the thermometer, as it was raised over a period of 2-3 hours to 103-104 C and held at that temperature for a further 6 hours.
5. After the 6 hour period the amber colored fluid was QUICKLY poured into a large beaker and allowed to cool to room temp.
6. When room temp was achieved, the beaker was noted to have a large amount of precipitated NH4CL. This was quickly filtered offf via Buchner and the remaining distillate was returned to the standard distillation rig. The NH4CL can be placed aside for future use.
7. The heat on the distillation rig was raised and half the liquid volume was distilled off.
8. The contents of the 3 litre 3 neck flask were again QUICKLY poured into a beaker and allowed to cool to room temp, and the distillate was discarded.
9. Upon reaching room temp the contents of the beaker had again precipitated a good amount of NH4Cl. This was again vacuum filtered via buchner and the NH4CL placed aside.
10. The remaining distillate was placed into the 2 litre R.B.F. and the 1 litre R.B.F. was set up to recieve.
11. Standard distillation was again commenced and a third to a half of the volume of the amber liquid is distilled Off until a skin has been noted forming. Then turn off the heat.
12. The contents of the 2 litre flask were QUICKLY poured into a beaker that was sealed with cling wrap. The contents of the 1 Litre recieving flask were discarded.
13. The beaker was allowed to sit for a few hours until room temp was achieved and then moved into the refrigerator.
14. After several hours the beaker was removed to the freezer and left overnight.
15. Next morning, vacuum filter crystals.
16. Dry vacuumed crystals are then covered in DRY acetone and swirled for several minutes and then Vacuum filtered again.
This step may not be necessary if temperature was correctly held at 103-104 for recommended time. Weight of crystals has never altered after acetone washes.
17. Store in a tightly sealed container.
Never less than 330 grams of Methylamine Hydrochloride (~4.9 moles, enough to aminate 290-300 grams MDP2P
), from 560 grams Hexamine, achieved with this method
The illegal we do immediately. The unconstitutional takes a little longer.- Henry Kissinger
(Stranger)
02-20-04 08:15
No 489990
Ok So Swim separated the white crystals from the methanol and froze the methanol thinking Methylamine should fall out of solution, but nothing happened. Did Swim mention my Hexamine was a year old and so was the Muratic Acid. Although neither of them had been opened. Help!!
(Old P2P Cook)
02-20-04 10:02
No 490014
This sounds like an odd method. If you will post a link I will provide commentary. How long did you maintain the reaction at 103°C?
All those moments will be lost in time, like tears in rain.
(Stranger)
02-20-04 11:06
No 490018
../rhodium /eleusis
Under hydrolysis of Hexamine. I started at the adding 140gms of hexamine to the acid. I also didnt used any heat during the 16 hr mixing period. It doesnt say to.
(Stranger)
02-20-04 15:06
No 490059
Ok so Swim separated the NH4CL form the methanol and took the methanol and tried freezing at lower temp -40 c. Still no precip. So Swim got a baking dish, poured the methanol into the dish and reduced it with a little heat. As it reduced it made the same skin over the top and gradualy got thicker. Now heres the fucked up part... Swim tilted the dish to check consistency and the fucker broke spilling all of the semi-solid crystals all over the floor. Anyway Is the shit on the ground the methylamine HCL. Is NH4CL not soluable in methanol and methylamine is??
(Old P2P Cook)
02-21-04 22:36
No 490334
I doubt that this procedure ("Hydrolysis of Hexamine" by Eleusis) works. I have written extensively here about the preparation of methylamine from ammonium chloride and formaldehyde (or paraformaldehyde) and also about the equivalent preparation using hexamine and hydrochloric acid in place of ammonium chloride and formaldehyde. The reaction has to be heated for a number of hours at 103-104°C or you will not get any methylamine.
All those moments will be lost in time, like tears in rain.
(Newbee)
02-22-04 00:40
No 490344
ammonium chloride and formaldehyde, how badly does this method smell. I performed a hex to methylamine, and boy did the place stink. Any Ideas on how to keep the smell down?
(Old P2P Cook)
02-22-04 12:21
No 490426
I performed a hex to methylamine, and boy did the place stink. Any Ideas on how to keep the smell down?
Neither method should produce any smell. What did you do that produced a smell?
All those moments will be lost in time, like tears in rain.
(Newbee)
02-22-04 13:18
No 490438
Hex to methylamine at first brought tears to the eyes, i guess it was formaldhyde, then during distilling smelled like stinky fish, you know methylamine.
(Hive Bee)
02-22-04 14:38
No 490451
ive done the hexamine to methylamine a few times it sucks
bad not a good way to go in my mind.
ive heated and also done it without heat both seemed to
work though the heated one did produce more.
as for were are my crystals question well there is a lot
of water in your mix methylamine is hydroscopic.
try using an amalgum on nitromethane in the solvent you
want the methylamine in use the smallest amount of water
you can use to get the amalgum to work. if you use methanol
you can probably do this anhydrous as I have heard methanol
will make the Al(OH) as well as water.
this way smells a whole heap less.
as for the hexamine method I find evaporating all of the liquid till I get a mush is the best though I would sugest
doing this under vacume aspirator as the shit stinks.
e3500 console login: root
bash-2.05#
(Newbee)
02-23-04 11:17
No 490627
yea, ive done hex to meam, ammonium cl and formaldehyde to meam, i used nitro for am, i tried them all, they all stink, but now im into hydroxylamine.
(Wonderful Personality)
02-23-04 13:47
No 490655
Ever heard of "condensor" and "distillation" ?
Of course if you just evap the shit on a hotplate in a frying pan you will have stink and poisonous fumes. One of the rare moments in life when there is an instant penalty for lazyness. To lazy to rig up a simple distillation setup = stink and obnoxious fumes inhaled, freedom is risked, health is damaged.
Done right there is NO, nada, zero, null stink. Period.
If there is stink it isnt done right. Period.
Eleusis may burn in hell for bringing up this "evap on the stove in a frying pan" BS. Probably one of the fabelous wanker jokes of our "english major".
Not to be misunderstood - I believe Eleusis being a far better chemist as the Yogis and Rhodis will ever admit - and he shared a lot of his best methods - thanks for this.
(Hive Bee)
02-24-04 10:11
No 490825
Regarding the methylamine synth with hexamine. If your in a pinch and you need meam right away from OTC stuff...it might be worthwhile go the hex route. The acetamide route requires way too much manual labor. The Nitro is nice if your a bit lazy, have large glassware to run everything in, and have a gallon of it stockpiled to use. The problem with nitro is that if you are planning on snagging some on the web there is a whopping selection of about 3 places who send anywhere..and have single gallon sizes. A while back there were more of them who sold no problem. Recently though something happened either with terrorism or ilegitimate uses or something but these same places will now only ship to commercial addresses and make you jump through hoops just to get the stuff. I guess once you have it your set..but IMHO MeAm.HCl made from 37% formaldehyde and ammonium chloride is the best way to go. Advantages.. the base chems required to perform the RXN are dirt cheap. The synth is basically "set-it and 4-get it" once you find your hotplate sweet spot. Workup is easy..and as long as you dont go over 110 while its in the 4-hour processing phase you will form minimal dimethylamine. There is a misconception here that the Methylamine smells like fish. The reality is the MeAm actually smells more ammonia-like. Its the DImethylamine which smells like stank fish. You usally get this when you over distill the mother-liquor (high-heat) and the DImethylamine starts to form and promptly vaporize. The absolute best part about using MeAm is the ability to use a small flask when you go to aminate. 55g easily reacts in a 1L flask. Also, if you wash your MeAm with chloroform (like your supposed to) the amination is actually cleaner than the nitro route. This is apparent at the end of the RXN when the oil separates and is visibly sparkling clear as well as the toluene after the extractions. Anyway, Im talking way too much here about silly MeAm. Just do what works for you I guess..
The shortest distance between two points is a straight line
(Wonderful Personality)
02-24-04 13:51
No 490864
I want to allow myself to link to this post of mine:
Post 488683 (Organikum: "For the vindication of Eleusis - Methylamine", Methods Discourse)
Please read the whole thread - nice picture in one of the followup posts!
These ratios:
100g hexamine
100g water
310g HCl 30%
100g ethylalcohol denat.
20g ammoniumchloride
Extraction by IPA yields 120g+ methylamine.HCl in clear colorless crystals (theory: 145g).
Washing with chloroform showed that dimethylamine was only present in traces if at all.
Hexamine is a charm in my opinion as it represents an ultracompact nonsmelling unsuspicious source of formaldehyde and ammoniumchloride (1mol hexa with 4mole HCl gives 4mole ammoniumchloride and 6mole formaldehyde... whatta want more?)
The ethylformate produced (about 3mole per 1mol hexamine) dissociates in water into EtOH and formic acic, but who needs formic acid....
Please dont poison yourself and your environment with this frypan-evap-shit procedure. It is a simple reflux/distillation setup for clean product and zero smell.
(Hive Bee)
04-06-04 07:50
No 499348
Hi! I made two times MeAm from hexamine and my second try worked very good, about 75-80% yield. The first time i was a little bit tired, that's why i forgot to add the water to the hexamine, before adding the Hcl. Refluxed for 6 hours (just hexamine+hcl), during cooling a lot of NH4Cl pricipated out. I saved all the reaction content.
My question is, will further processing result in some MeAm, or should i just filter out the NH4Cl and discard the rest? I've read, that it doesn't work without water, that's why i'm asking. greetings
(Hive Bee)
06-09-04 16:48
No 512501
Actually, I too made the mistake of forgetting to add water (just alcohol, hexamine and acid) - noticeable exotherm reaction, placed it in a water bath and was just about to start slow heating - suddenly I remembered there was still a reactant missing! I then added the water immediately, continued as if nothing had happened (2h reflux, 3.5h distillation of ethylformate, reflux 1h, alcohol removed using vacuum) and got still good yield...
(but also got some strange white substance, insoluble in acetone/alcohol/water - it appeared after alcohol removal, was filtered and found to be hard, crunchy and not crystalline. I suspect it to be something similar to hexamethylene(triperoxide)diamine or HMTD, see also Post 512495 (armageddon: "explosive by-product?", Methods Discourse)
Greetz A
"..ein Trank von unterschiedlicher Farbe, in ihm ist Heilung für die Menschen."
(Hive Bee)
06-16-04 01:07
No 513748
This seems to be the right thread for posting this:
Methenamine
CAS 100-97-0; 587-23-5; 5714-73-8
(Formamine, Hexamethylenetetramine, HMT, HHMTA, Methenamine, Urotropine)
full name: 1,3,5,7-tetraazatricyclo[3.3.1.13,7]decane
or: 1,3,5,7-tetraazaadamantane
Made by reacting formaldehyde and ammonia:
6 CH2O + 4 NH3 ---> HMTA
see also Patent US2763799 and Patent US2762800
Hexamine is commonly used as an urinary antisepticum, and it is sold under the brand names:
Aci-Steril, Antihydral, Hiprex, Mandelamine, Prioherp, Urotractan (germany)
Aromalgyl, Formocarbine (france)
Hiprex, Mandelamine (GB)
Elmitolo, Jodoibs (italy)
Hexamine (japan; they apparently don't like trade names
)Uro-Phosphate, Hiprex, Urex, Mandelamine, Thiacide, Uroquid-Acid (USA)
In case you dislike your pharmacist
:Well branded fuel tablets are said to contain 99.9% hexamine, too...
..and are WAY cheaper..
Greetz A
"..ein Trank von unterschiedlicher Farbe, in ihm ist Heilung für die Menschen."