Author Topic: Chromic’s Methylamine.HCl  (Read 4782 times)

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RoundBottom

  • Guest
Chromic’s Methylamine.HCl
« on: June 20, 2002, 02:34:00 AM »
this is a repost from a somewhat obscure thread in the newbie forum...

Post 322683 (missing)

(RoundBottom: "Chromic’s Methylamine.HCl", Newbee Forum)
  i don't think it was as visible as it would be in it's own thread, so here it is.

Written by RoundBottom (karma, money, sex belong to chromic)

Preface:
First, this is a first attempt at making any MeAm.HCl so what it is supposed to look and smell like is a complete unknown (but whooee bob stinky-twat smell is bang on).  Second, RB really knows nothing about chemistry other than what RB has learned since attending the Hive.  Also, RB has never written a lab report in his life, so if the format is really off, please make any needed edits.

Reagents:
· 179.7g Hexamine camping fuel tablets
· 500mL muriatic acid (31.45% HCl acid)
· 550mL MeOH
· 550mL Acetone

Apparatus:
· 1L distilling flask
· 500mL receiving flask
· standard distillation setup (with cooling)
· rubber hose
· 600mL beaker
· 1000mL beaker
· 1” egg stir bar
· stir plate
· mantle and controller
· filter flask
· Buchner funnel and stopper
· filter paper
· vacuum source

Notes:
· The white hexamine tablets were a very common, “green Canadian camping products” brand.  The tablets were put into a baggie and crushed to fit into a 1L flask. 
· Chromic’s write-up suggests mixing the muriatic acid with the Hexamine in the flask while it sits in an ice bath.  No temperature increase was noted, so this may be unnecessary.

Procedure:
Set up distillation apparatus as usual.  A rubber hose was run from the vacuum inlet on the vacuum adapter to a window to expel any fumes. 

Mix the muriatic and hexamine until dissolved.  Took about 15 minutes, but will vary depending on hexamine type.

A gentle reflux was maintained for about 7 hours at a temperature of about 80°C-85°C.  The heat was turned up to start the distillation.  Fluid started dripping into the receiving flask at about 102°C.  At about 11.5 hours, grains of AmCl were observed mixing in the distillation flask.

After about 12.5 hours the temperature had raised to 107°C and the drip rate had slowed down to about 1 drop per 4-5 seconds.  About 270mL of clear distillate was recovered.  It shouldn’t be required and can be disposed of later.

The heat was turned off and the reaction contents were allowed to cool down while still stirring.  The fluid in the distillation flask had a medium yellow colour to it, and was still clear.  There was also a large amount of spongy looking solids in the distillation flask that did not harden after cooling down, but remained sort of mushy.  Bubbles were still evolving even after the distillation flask was allowed to cool for about 45 minutes.

A note about smell: once the distillation flask was removed the smell was really evident.  It will stay in the room and on the skin for a few days.  If you can at all manage it, make a fume hood, do this outside, or at least with a fan blowing out the balcony door.  Smelly-twat, rotten anchovies, smegma dick… take your pick, it’s pretty nasty.  Don't expect to hold a dinner party there the next day.  The rubber hose is only useful while the distillation apparatus is connected.

Once cool, the contents of the distillation flask were vacuum filtered with saran wrap to squeeze out as much liquid as possible.  About 250mL of fluid was collected (murky and cloudy, dark urine coloured).  The crystals were put into the 600mL beaker and covered with 150mL room temp MeOH, manually mixed with a spatula for about a minute, poured into the filter.  The beaker was rinsed with about 50mL MeOH and poured into the filter funnel, and then vacuum filtered, again with saran wrap.  The AmCl crystals were put on a Pyrex dish to dry and kept for future use.  Once dry, the ammonium chloride weighed 104g.

The combined filtrate and MeOH washes were then put back in the distillation flask, and distillation was started again.  A temp of 40°C was reached in 25 minutes and fluid started coming over (BP of MeOH == ~64.6°C)

The temp climbed up to 108°C over 5.5h.  After about 300 minutes a white smoke started filling the distilling flask.  This is what we are waiting for, the sublimation of the MeAm.HCl.  "Distilling to dryness," means the flask doesn’t have any more water in it.  It does not mean, "Boil the hell out of it till everything's crunchy"

Once the smoke appeared, the heat was turned off and the contents were left to cool and solidify for 30 minutes.  Sorry, the appearance of the fluid at this point wasn't noted.  Once cool, 350mL MeOH was poured into the distillation flask and a reflux condenser was put on the flask (actually, the condenser from the distillation phase can be used, as it is already set up and this isn't a heavy reflux).  The heat was turned up again, and the solution was allowed to reflux for about 15 min.

While hot, the solution was decanted into a Pyrex dish (a 1000mL beaker is probably better).  Either way, the container was covered with saran wrap and left on the counter for 2 hours until cool.  It was then moved to the fridge and left overnight.  In the morning the beaker was moved to the freezer for another 2 hours.  The crystals were large crunchy flakes, and the remaining fluid had an amberish tint. 

It was once again vacuum filtered with saran wrap.  About 375mL of fluid was recovered.  At this point the crystals were large, white, translucent, and crunchy. 

The crystals were put into a 600mL beaker and washed with 200mL ice-cold acetone for 5 minutes, and again vacuum filtered with saran wrap.  The crystals were then spread out in a Pyrex dish to dry.  The crystals looked smaller, and had a slight grayish tint. 

The remaining fluid was crashed with 300mL ice-cold acetone and about 1.5g of crystals fell out.  It was decided that it wasn't worth boiling the liquid down to recover any more.

In total 98.2g of crystals were recovered. 

 


i learned a thing or two from charlie dontcha know.

Rhodium

  • Guest
Where is Chromic's original writeup
« Reply #1 on: June 20, 2002, 02:51:00 AM »
Nice, Nice... Where is Chromic's original writeup, BTW? I can't find it on my page  :P

RoundBottom

  • Guest
dunno
« Reply #2 on: June 20, 2002, 02:58:00 AM »
he passed me an early version, but said he wanted to tweak it a bit.  that was a few months ago, so i decided to post my report of his writeup.  i think he got busy and forgot... but i'm sure he'll be posting it here, soon.

i learned a thing or two from charlie dontcha know.

Chromic

  • Guest
Original writeup
« Reply #3 on: June 20, 2002, 10:01:00 AM »
The original write up is on the Hive. The only real difference is the use of MeOH to recrystallize followed by washing with acetone.

The main advantage over the other MeAm.HCl writeups is the reduced solvent volume necessary to recrystallize. I found using IPA was a slow and tedious way to recrystallize. I hated using IPA or any other higher alcohol than MeOH (and hated washing with DCM), so I looked for solvents that would give a good purity of MeAm.HCl. MeOH was found and it worked wonderfully.

I also noted that the reaction does not take place with the solution at 104°C like other bees indicated. It takes place at a slightly higher temperature (the temp of the vapor, however, is 104° at the beginning). As I never repeated this synthesis more than 3 or 4 times I never released a final copy of my write up.

The yields are lower than other write ups (typically 50%, but sometimes lower), but it's so easy and the purity is so good, these two factors were never an issue. The key to getting a good purity is allowing the MeOH to cool very slowly and undisturbed. MDMA made with this MeAm is highly quality stuff too, I doubt there is much dimethylamine left in with the crystals. Btw, reducing the MeOH volume used might increase the yields... but I never experimented with it. (I just used amounts that I determined semi-quantitatively from my work recrystallizing MeAm.HCl... details found in other posts)

Good work RB! You finally brought this method to the public.  :)

pROcon

  • Guest
Excuse me, sorry for invading this thread with my ...
« Reply #4 on: June 21, 2002, 01:25:00 AM »
Excuse me, sorry for invading this thread with my minimal chem skills, but does this have any relevance to the smelly aldehyde E-quest murmering?

A myth was formed somewhere along the line - that Americas government is not the fault of Americans.

GOD

  • Guest
binders
« Reply #5 on: October 24, 2002, 02:21:00 PM »
If the hexamine source (E....) is known to have binders in it, is it first nessisary to remove them before performing this rxn?

Loriel... because Im worth it!

Rhodium

  • Guest
That's a good thing, as you don't know what the ...
« Reply #6 on: October 24, 2002, 03:04:00 PM »
That's a good thing, as you don't know what the binders are. They are usually not water soluble.

RoundBottom

  • Guest
example
« Reply #7 on: October 24, 2002, 07:11:00 PM »
the hexamine tablets used in my example were well formed pucks about the size of a quarter and about 1/2" thick.  when struck with a hammer, they easily crumbled to powder. 

Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)

ChambeRed

  • Guest
I've tried two different brands of hexamine ...
« Reply #8 on: October 25, 2002, 07:18:00 PM »
I've tried two different brands of hexamine tablets and bolth seem to work just fine,they bolth come just like chromic described.Pm me if you doubt yours for a sure thing.Peace,Chambered.

Bee's don't die,we just multiply.

Diggity

  • Guest
?>
« Reply #9 on: October 25, 2002, 08:04:00 PM »
What is the brand name of some good working Hexamine tabs? I have yet to try this method, and am feeling a bit bored this afternoon. Thnx,

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

Chromic

  • Guest
Any of them
« Reply #10 on: October 25, 2002, 08:49:00 PM »
Any of them will work. Make sure they're white, hexamine and crumble apart. Chromic had good luck with the yellow and black packages, but the blue and whites ones work too. Go out & look.

GOD

  • Guest
clarification
« Reply #11 on: October 30, 2002, 08:53:00 PM »
Set up distillation apparatus as usual. A rubber hose was run from the vacuum inlet on the vacuum adapter to a window to expel any fumes.
...
A gentle reflux was maintained for about 7 hours at a temperature of about 80°C-85°C. The heat was turned up to start the distillation. Fluid started dripping into the receiving flask at about 102°C. At about 11.5 hours, grains of AmCl were observed mixing in the distillation flask.


This means to set up for simple distillation, or is a fractionating column used?  Swim ASSuMEs this to mean simple distillation, but since a reflux is mentioned...

BTW, those E**** brand cubes (come in a red box) definatly come with a binder in them, recrystalisation of 2 boxes (12 X 14 grams/box) yielded 329.7G hex. and ~6G hard, semi-waxy binder.

Loriel... because Im worth it!

RoundBottom

  • Guest
simple
« Reply #12 on: October 30, 2002, 09:14:00 PM »
you are correct, simple distillation.

i've only used one brand, and there isn't much in the way of binder.

Now with 12% more Bottom!
Nymphomania is not a disease, its a goal! (Methadist)

Chromic

  • Guest
Red box hexamine
« Reply #13 on: October 30, 2002, 10:03:00 PM »
Yes. The german brand has got a wax binder in them and this has been discussed before. Do not recrystallize your hexamine. The content of binder is very low (I think someone even had a web page up with pictures on this topic), so just throw them into the flask (they even fit, unlike the black & yellow box which you have to smash up).

The methanol recrystallization will not take any of that binder into your purified methylamine.

Is anyone else paying out the ass for these things? They cost me ~$15US for ~250g. Oh well, it turns into 100-125g of methylamine, so I guess it's all good.

GOD

  • Guest
$4.99 US for 168G/box
« Reply #14 on: October 31, 2002, 12:08:00 AM »
$4.99 US for 168G/box

Loriel... because Im worth it!

ChambeRed

  • Guest
2.99 a box and 144g. a box and with no noticeable ...
« Reply #15 on: October 31, 2002, 04:44:00 AM »
2.99 a box and 144g. a box and with no noticeable binder,Sta*sp*r* brand.Found it a the "action figure/cartoon hero)" sporting goods store.

Bee's don't die,we just multiply.

majic22

  • Guest
vacuum filtraion with saran wrap?????????
« Reply #16 on: October 31, 2002, 07:42:00 AM »
this may sound like a dumb question but ive always been told the only dumb question is one not asked so here goes...where does the saran wrap come in?  I have a basic understanding of vacuum filtration but i dont understand how you "vacuum filter with saran wrap"  thanks

"My girlfriend said I had to choose between her and chemistry....Im gonna miss her."

raffike

  • Guest
I paid something like that: 12$ for 35 kg bag of .
« Reply #17 on: October 31, 2002, 12:43:00 PM »
I paid something like that:
12$ for 35 kg bag of AmCl and
6$ for 33 liter canister of Formalin.
and i don't feel like being ripped off.
I once tried that Hexamine to methylamine synth but it was very time consuming and low yielding for me.I'm completely satisfied with AmCl/Formalin synth.

A friend with speed is a friend indeed

Chromic

  • Guest
Saran wrap
« Reply #18 on: October 31, 2002, 03:55:00 PM »
The saran wrap pushes down on the crystals to get more solvent out. Just put a piece over the buchner funnel when you're done pouring the slurry thru the filter. It gets sucked to push on the crystals by the vacuum.

uncle_buck

  • Guest
A suggestion or three...
« Reply #19 on: November 07, 2002, 07:10:00 PM »
Great write-up!

Some quick suggestions/observations:

1.  purchased hexamine powder gives better results, this is based purely on personal observation

2.  ammonium chloride can be rextallised from boiling water and feed into more methylamine production thru the route with (para)formaldehyde, thus upping yield

3.  rextallising methylamine.hcl from isopropyl alcohol instead of methanol gives cleaner results, again based on personal observation only

cheers!

ub