01-31-01 22:21
No 170447
For those who can't get their hands on a sufficient amount of gaseous Methylamine, what would be the method of choice to make it in sufficient amounts themselfs, fast and easy, without any difficulty to obtain precursor chemicals and/or complicated machinery?
Lets look first at these 2 threads :
Post 72966 (Elvium: "MeAm in MeOH for NaBH4 reductions", Novel Discourse)
MeAm in MeOH for NaBH4 reductions Hive Novel Discourse
Post 81703 (Methyl_Man: "Methanolic MeAm via Al/Hg/MeNO2?", Novel Discourse)
Methanolic MeAm via Al-Hg-MeNO2 Hive Novel Discourse
and then two simple methods prevail :
1. Formaldehyde + Ammoniumchloride --> heat 4 hrs at 105 °C --> MeAm in huge batches.
2. Hexamine + HCl under vacuum refluxing.
I would like to have a memorable writeup from anyone who has experience with both methods, or any other method which falls in this category.
Any link to past writeups is also welcome, I remember vaguely that we had quite some discussion going on on both subjects, 1 in the newbee forum in the very beginning of the forum, and 2 also somewhere there and prolly a lot of posts in other forums.
It's time we compile all this info in this thread, and then I can place it in the sticky thread on top of this forum.
We have much to much shattered pieces of important info lying around in numerous forums, its time to compile all that badly needed MeAm gas info in one place.
There is also a long forgotten easy method of making small or huge amounts of MeAm gas starting from MeNO2 (nitromethane, methylnitrite), carefully warming it up in a vessel where a vertical glass or metal pipe is placed on top of it, filled with an oxidized Nickle wool catalyst and a heater-coil around the pipe, there where the Nickle-wool sits, and introducing a small stream of H2 gas just under the Nickle-wool to start the conversion to MeAm gas.
The MeAm can then directly be bubbled in to a cooled container with dry methanol. This can be converted to a continuous operation, see the huge picture?
The tricky thing seemed to be the necessairy oxidation of the Nickle-wool catalyst to a black colour, but not overly difficult, perhaps sending a amperage of sufficient power through a coiled Nickle-wool to red hotness in a container with oxigen will do the trick. Or just heating it in a gasflame feeded with oxigen also, and then dispersing it in a beaker filled with oxigen, until the oxigen is used up, and the wool is blackened.
Anyone having ideas about this procedure, please feel free to hop on this thread too. LT/
WISDOMwillWIN
(Daddy)
02-01-01 13:16
No 170595
British Patent 203218 about Lush catalyst, oxidated nickle wool LT/
WISDOMwillWIN
( )
02-05-01 08:25
No 171262
Ye have only to ask and ye shall receive.
The adventures of da na na na na NOT-CHEMIST!
Title: The scale-up
This is an essay on how not to make methylamine. It is the hypothetical story about the second time a not-chemist decided to make a batch of Methylamine. After all, it was soooooooo easy the 1st not-time at a 1/5th scale.
The not-proceedure (how to gas yourself)
A 4l erlenmeyer flask sitting on a hotplate, is charged with 2500g formadehyde and 1250g ammonium chloride. It is then stoppered with a two holed stopper. In one hole a thermometer extending into the rxn mixture, in the other a glass tube attatched to a rubber hose leading out doors. Heat is applyed bringing rxn temperature to 104deg C over a 1hours period (lunch time). As temperature approaches 104C the ammonium chloride goes into solution, and a vigourous reaction begins. The not chemist decides to have one last peek before returning to work in the afternoon. Fuck! the rxn has blown the stopper out of the flask, and this horrible smelling gas fills the room GAK! Anyways the damned stopper won't stay in the flask it just keeps blowing out, Choke, cough Gakk! The not-chemist is starting to feel very unwell. On with the gas mask. finally using a broom handle wedged against the ceiling he is able to get the stopper to stay in the flask. Off to work for one very unwell feeling chemist.
(how to gas yourself again and wreck half your lab equipment)
After work (4hrs later) the flask is heated more allowing half the volume of the rxn to boil off. The flask is cooled and the precipitation of ammonium chloride is vacuum filtered off. (Keep this for next rxn) The filtrate now able to fit in a 2l flatbottom flask. Is returned to heat in a vacuum distiilation set-up. Heat is applied with low vac (rootary vane pump). Later that evening the not-chemist notices this bad smell. Goes and has a look. the flask is boiling uncontrollably, going wild! Upon closer inpection he realizes that the bottom of the flask has imploded and shit is spilling all over the place. As the chemist lifts the cracked flask into another container the rxn spills all over everything (inclyding the hotplate,) making huge fucking clouds of methylamine gas and formaldhyde FUCK!!!!!!!. Gas mask comes back on, damn these things are heavy and after about thirty seconds you can't see fuck all cuz of all the condensation. So sweating like a bastard in this gasmask and toxic fume infested lab. The mess is cleaned up. Finally get the remains of the rxn thing going on hotplate #2 (hotplate #1 friied during implosion, shorted out with electricy cutting a hole through the housing on the motor!) Also when the thing went nuts it sucked all kinds of shit into the vacuum hose, filling the vac pump with formaldehyde and Methylamaine, ruined vac pump!
(the only uneventful step)
Things are reduced by 50% again and another load of ammonium chloride crystals is filtered off. Then it is reduced some more until things spontaneously crytaliiize in flask. Finally the methylamine! This is filtered off, and the filtrate, further reduced and more Methylamine filtered out. This crude Methylamine is recrystallized out of boiling n-butyl alcohol 3 times. Then washed with chloroform to remove any dimethylamine (sp?).
(how to go bald and burn your fucking house down)
Get ready here comes the icing. The following lunch hour the chemist wants to wrap this up, but crystals look a little soggy, so the not chemist decides to put em in a pan in the oven to dry. After 20 minutes at 200C they don't look any driier. so chemist cranks the heat to broil and goes back in the lab. His first clue that something is amiss is when the smoke alarm goes off, Aw fuck here we go again! The not chemist returns to the kitchen to see the oven engulfed in 4foot flames, MOTHER OF JESUS! With no regard for personal safety the chemist opens the oven door (Like wtf else could he do?) Thing bursts into renewed flames (ARGGGGG!) anyways accompanied by the smaell of burning flesh (chemsits fingers) and scortched eyebrows the pan is removed to the back porch, leaving scortch marks on the ceiling all along the way (howmagonnaexplainthatone?)
(epilogue)
After roasting marshmellows on methylamine fueled bbq for 5 minutes or so the chemist decides maybe something can be salvaged and thows another pot over top this one to extinguish the flames. (marshmellows tasted like shit!) Well there were certainly some losses along the way, but the not-chemist happily ended up wth something in the neighbourhood of 500g slightly scortched methylamine.HCl. Not bad for a destroyed 2l flask, vac pump, hotplate stirrer, stove and celing paint fingers and lungs.
Next episode, Mount St Helens: the not-chemist makes Al/Hg volcanoes!
Next month: Not-chemsts adventures with LAH
Re-runs: Not-chemist meets cyber wench.
Just gone.
(Daddy)
02-05-01 09:48
No 171264
That's one of the most memorable writeups I saw ! Reminds me of the chinese cooks with those huge woks, they let the veggies plus the cooking oil also burn repeatedly with lots of big flames.
This procedure is quite good described in Vogel's, where is that thread in the Newbee forum where I posted the whole Vogel procedure on how to do it the right way? Will do a search soon. LT/
WISDOMwillWIN
(Daddy)
02-05-01 10:21
No 171266
Post 123284 (LaBTop: "Re: Questions about MeAm formation", Newbee Forum)
That covers both methods I asked for, look for Chemhacks post in there for the hexamine/HCl method.
I totally forgot I posted all that info allready, well, here you have it back. LT/
WISDOMwillWIN
(Hive Bee)
02-05-01 16:41
No 171319
I printed this out before. It looks interesting. Post 108044 (beeach: "Methylamine in Methanol for the bromosafrole route", Novel Discourse)