## Synthesis of Methylamine

### by Zwitterion

Is it safe to take the gas mask off now??? I dunno, it's still pretty smokey in here! But whoa there, dogie! Look at that big, beautiful batch o' methylamine HCL! I mean, FUCK, there's enough here to... uh... well, there's a LOT. ZWIT, your ever fearless, ever intrepid, ever death-defying ChemSlave (tm), took the latest version of the Methylamine FAQ in hand (v.2.6) and looked it over. Soon, a thin stream of drool started flowing from ZWIT's gaping maw. There were two new targets! The nitromethane reduction sounded kinda fun, but ZWIT had the chemicals on hand to try the Hexamine crap, so what dafuck, right? This is the tale of my experience, learn from it, revel in it, repeat my success, and avoid my FUCKUPS. #### TRY #1 ZWIT was feeling extra careless that day, and extra greedy. I needed a big-ASS batch of methylamine, and let's face it, that pathetic Hofmann crap is as much fun as using GoJo with pumice to jack off. So ZWIT dumped 250mL of stink-to-the-hig-heavens 28% ammonia into a glass beaker near a window with a FAN. By god don't try this without SERIOUS VENTILLATION, ok? Next, ZWIT measured out 490mL of 37% formaldehyde solution (where da fuck does E get 40% from??? Little bastard!) which is still SLIGHTLY LESS FORMALDEHYDE THAN AMMONIA (mole-wise). ZWIT casually started pouring the formaldehyde into the ammonia and things were looking kinda nice when all of a sudden! Boom! A great eruption of nasty vileness sprung from the beaker, spraying all of me and my kitchen with the shit! Holy-freakin-frijoles! Off to the shower I went, and then spent the next two hours cleaning everything in my kitchen with a gas mask on - damn those things get HEAVY after awhile. The moral of try #1 - ADD THE FORMALDEHYDE SLOWLY!!!!!!!! #### TRY #2 Alright. I was feeling a little SCARED from the first experience, so ZWIT decided to PAY ATTENTION this time. ZWIT also decided that maybe a half-size batch would be better, so 125mL of 28% ammonia goes into the beaker near the window fan and 245mL of 37% formaldehyde was measured out. ZWIT slowly adds the formaldehyde and nothing exciting happens until about 2/3 has been added. Then the shit starts bubbling everytime I add just a smidgen. ZWIT stirs like a madmen with each 10mL spurt added and finally all went in without a hitch. The solution ended up pretty warm, but looked stable, so ZWIT dropped in a stirrer magnet and let it spin happily away for the next 16 hours or so. If you thought that was exciting, wait, cuz it gets even BETTER. ZWIT then dumped the clear solution, which had this peculiar odor unlike either formaldehyde or ammonia (ZWIT takes this as a GOOD thing), into a stainless steel frying pan sitting on top of a 5 quart boiler half-filled with, you guessed it, water. ZWIT used this half-assed apparatus to evaporate all the water out of the frying pan, making loads of isocyanate-like fumes! This shit is NASTY, lemme tell yah. Once again, it was absolutely neccessary to don the ole gas mask. Within an hour or so, with occasional stirring to keep everything from popping and fizzing too much, there was a nice crop of slightly damp white needle-like crystals. Don't get the nose/eyes too close to them, the vapors are not pleasant. ZWIT weighed them out and got 75g, which considering they were damp, meant that I got a quantitative yield - just like E says, how nice. ZWIT didn't bother to dry them any further, he just dumped the entire shebang into 200mL of 31.5% HCl (the pool shit). There was no excitement involved here, and the temp of the solution just barely rose. ZWIT didn't know how important stirring was to the whole process, so he just dumped this solution into the same old frying pan on the same old 5 quart saucepan and evaporated away. Whoa! Those fumes are KILLING ME, MAN! It looked like things were going real slow, so ZWIT placed the fry pan directly onto a burner at LOW heat. After a total of 5 hours, with the stuff still looking like mush, ZWIT gave up and set the fry pan aside to cool. When ZWIT returned, the crystals where much drier and chunkier! ZWIT was actually SUBLIMATING the methylamine HCl when he thought it just wasn't dry! Now wonder the shit changed from smelling like HCl to smelling like, well, burning crotch! The crystals were white with just a hint of yellow - they really didn't look like the reagent grade of methylamine HCL. No surprise here, considering my kitchen is NOT ACS APPROVED. Anyway, it didn't look the same as the hexamine shit, but I wasn't entirely trusting it was methylamine HCL either. I took a chunk and tried to dissolve it in acetone, which Hexamine IS soluble in, but methylamine HCL ISN'T. The shit DID NOT DISSOLVE - a very good sign indeed! ZWIT took a crude yield, and if things had gone quantitatively, I would have had 135g of methylamine HCL, but since I let it sit on the burner so long, I only got 100g. Oh gee.. only 100 freakin' grams! Hah! Why, I'd have to do THREE freakin' Hofmann batches to get that kind of quantity! Fuck yeah! ZWIT dumped all of the crystals into a beaker, covered them with acetone, and started chopping and smashing away so they'd be nice and fine. ZWIT then dumped the whole mess into a buchner funnel and sucked off all the acetone by laying a piece of saran wrap on top of the filter cake so it'd get good and vacuum packed (for freshness). ZWIT quickly spooned all of the filter cake, which was a brilliant white deliquescent powder, into a glass container. Crystals that were left behind quickly soaked up water from the air and turned into little puddles here and there, JUST LIKE METHYLAMINE HCL OUGHT TO DO, and unlike what Hexamine does (it just sits there, happy to be dry). All in all, the process seems MUCH more viable than anything else E has come up with, and ZWIT gives it a 3 star (out of 3.141579) rating. The crystals aren't colorless like reagent grade methylamine HCL, but when you drop a gram of it into some dilute NaOH solution, it sure stinks like methylamine! ZWIT'll let y'all know what happens when it actually gets USED in a batch. Hah! One last thing... the formaldehyde cost me $45 for a gallon, the ammonia cost about $35 for a gallon and who cares about the HCl ($2) - all purchased locally. Since formaldehyde is the limiting reagent, this means for about $80 I can make over a kilogram of methylamine HCL. How 'bout them apples? [END OF TRANSMISSION]
    Subj: *ZWITTERION* - Consults the Holy Amine FAQ, Receives the Divine Manna
    From: eleusis@netcom.com (Eleusis)

    > I took a chunk and tried to dissolve it in acetone, which Hexamine IS soluble in,
    > but methylamine HCL ISN'T. The shit DID NOT DISSOLVE - a very good sign indeed!
I don't know where ZWITTERION got this information from, but I have no data on whether hexamine dissolves in acetone or not. I do know that it is soluble to the extent of 3 parts to 100 of hot absolute ethanol, and that methylamine HCl is soluble to 23 parts in 100 of the same. Acetone is probably an ineffective wash solvent, and solubility characteristics for similar alcohols can be inferred from absolute ethanol (ie - one would expect methanol to more effectively dissolve methylamine HCl than hexamine just like abs. ethanol).
    > All in all, the process seems MUCH more viable than anything else E has  come up with,
    > and ZWIT gives it a 3 star (out of 3.141579) rating. The crystals aren't colorless
    > like reagent grade methylamine HCL, but when you drop a gram of it into some dilute
    > NaOH solution, it sure stinks like methylamine!
Gee, nice to see my work has been approved by the world's worst home chemist ;-). At any rate, it appears this is the best qualitative test for quick and dirty identification. Methylamine has a very, shall we say, "distinctive" smell. I am unsure of what would result in the white form of the product, except that is possibly the anhydrous form. Allowing it to stand in air, in a finely divided form, will probably result in it hydrating enough to turn colourless. It will eventually deliquesce, though. Sounds good to me, though.