Boomer Posted March 22, 2006 Posted March 22, 2006 On my search for a melt/cast AN mix (see thread in HE) I kept looking for ways to lower the mp. AN/UN/HDN/NaN gets below 100C, but the HDN starts to stink already at that temp, especially since you first have to go above 100C to start the melting. Enough said, I settled on MAN (methylamine nitrate) which gives an eutectic with An that melts at 55C. MAN is CH3NH2.HNO3, made from CH3NH2 (methylamine) and nitric acid. Now where to get methylamine? It is heavily watched due to drug manufacture. Hence a look at Rhodium or The Hive gave many synths, mostly for the hydrochloride salt since the amine is a gas. First of all, Mr. Cools method did NOT work. Mixing hexamine and HCl, then driving the water off gave crap, most likely ammonium chloride. Instead of C6H12N4 + 4 HCl + 4 H2O --> 4 CH3NH2.HCl + 2 CO2 it probably went C6H12N4 + 4 HCl + 6 H2O --> 6 CH2O + 4 NH4Cl SHIT!!! An XTC folder from Rhodium included MeAmHCl as well, basically the same method but adding EtOH. It went like 140g hexamine + 400ml 31.5% HCl + 'at least' 100ml EtOH. The second difference is that you wait half a day before driving the water off, filtering the precipitate out that forms in that time. I waited a day, and can back up Eleusis' suspicion that it's paraformaldehyde that forms. So far: 8g hexa, 8ml denat. spirit and 24ml 31.5% HCl formed 3.5g paraformaldehyde over night. Half of the remaining sln gave 3g of slightly moist 'methylamine hydrochloride' (hopefully) on slow evaporation at 35C on the radiator. The other half will be boiled down to yield xyz g more (not finished). A funny thing is that in my drunk stupor, I FORGOT to make the nitrate, and used the hydrochloride in the melt/cast. M.p. was 55C as with the nitrate. Coincidence, or what the fuck have I made? Now please someone start threads about performic/peracetic acid oxydation and Al/Hg reductive amination?
Axt Posted March 22, 2006 Posted March 22, 2006 Your after "formit". Its in vol. 6 F172 of PATR2700. In brief, condense 6 moles AN with 6 moles 30% formaldehyde by refluxing 1 hour, dry in vacuum to recieve what I assume is OB'ed ratio of AN/MAN. (~70:30) though it lists a setting point starting at 90°C. Probably seen it already but searchin' PATR2700 for "Ammonex" (1, A293) will give other cast AN comps that use urea or NaNO3 to lower MP.
Boomer Posted March 24, 2006 Author Posted March 24, 2006 Thanks for the tip. But I am not exactly after formit, instead I want MeNH2.HCl and MAN as single species too. It's highly unlikely that I ever make E, from lack of lab equipment and also criminal intent. But having made OTC the lil sister of the Amines We Have Known And Loved is a challenge in itself. As far as the melt/cast goes, I went brute force and dissolved my (suspected) MeNH2.HCl in 53% HNO3 (1:1 molar), then boiled down and cooled. Even with HCl being stronger, it should evaporate and leave the nitrate. Result: Chasing the MAN dragon down a folded alu foil, it melted, then hissed at me and burned away more energetically than HDN, not half reaching the other side of the foil. Seems I got what I expected - what else can it be, nitro-formaldehyde, EDNA, MEDINA? Unlikely!This means the first stuff must have been the hydrochloride as I had hoped! P.S. Just found a better methylamine FAQ, Eleusis may know about E but Rhodium finally enlightened me. It' also on the Rhodium-mirror on designerdrugs.com, but hidden somewhere else.
Douchermann Posted March 30, 2006 Posted March 30, 2006 Methylamine isn't only used to make E, it's also used to make meth, using P2P with Al/Hg amalgam but I never said that You need to actually reflux the mixture, not just drive the water off. Supposedly, some formaldehyde is created during the reaction and a formaldehyde solution boils lower than water, or at least the 37% soln. does. If you're really desperate, I'm sure you can make a reflux column out of some 2cm glass tubing and ductape
Axt Posted March 31, 2006 Posted March 31, 2006 Sounds like you have what you were after. Anyway, attached is the article referenced from Rhodium, which is nice to have. As a test of faith, try chlorinating it to the explosive CH3NCl2. Any NH4Cl and you'll get NCl3 well, you could probably react it at a temperature high enough to prevent NCl3 accumulating as N,N-dichloraminomethane should be relatively stable, but still easily detonatable with a cap, at least if its at all simular to its ethylendiamine analogue.the_preparation_of_methylamine.pdf
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