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Organikum
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Ammonia and methylamine are both gases.
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Geomancer
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The nifty thing about gasses is that they become less soluable with temperature. Heat will drive a lot of ammonia out of solution. Same should work
for methylamine. Don't expect it to be quantitative, though.
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acx01b
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same with HCL aq: I expect that CaCl2 or MgSo4 would work to get HCL gaz...
but maybe im completly wrong.
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Organikum
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No you are right - and probably know this very well - heat, as CaCl2 and MgSO4 will drive out HCl - but the same as with ammonia and methylamine
driven out by heating you cant expect the gases to be anhydrous.
CaCl2 and MgSO4 wont work very well for ammonia and methylamine though. But you can form the salt, methylamine.HCl or respectivly ammoniumchloride and
drop an concentrated aqueous solution of the salt onto excess NaOH or KOH. This will produce the gas. If the NaOH or KOH is admixed with CaO -
quicklime - the produced gas will be fairly dry. Otherwise an dryingtube filled with NaOH or better NaOH/CaO will dry the gas completely.
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acx01b
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wow
nice
i'll try it tonight for the pleasure with my little equiment.
but to get some dried NH3 we can use hexamine too no? easier? (dont need to make dried NH4CL 1st)
[Edited on 8-5-2004 by acx01b]
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Organikum
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but to get some dried NH3 we can use hexamine too no? easier? (dont need to make dried NH4CL 1st)
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I guess you got something wrong here.
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If_6_was_9
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Has anyone considered this?
https://www.the-hive.ws/forum/showflat.pl?Cat=&Number=41...
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acx01b
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ty vm,
specially the links page's nice: https://www.the-hive.ws/forum/showtext.pl?Cat=&Show=link...
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Mendeleev
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I was wondering if the formaldehyde and ammonium chloride method could be done with lower concentrations of formaldehyde, such as 20% or 30%, by
adjusting the amount of formaldehyde added? What I specifically had in mind was could it be done campa-chem style?
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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Mendeleev
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Sorry for double postin everyone, I am on an old computer with an old browser and everything is very weird, but I just wanted to add one more
question, everyone says to distill the hexamine, HCl mix, but that's not really necessary unless you want to collect the biproduct right? You
really just have to mix, heat, evaporate off, filter, and recrystallize right?
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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Polverone
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How interesting! I believe the prep can be considerably simplified as well. Sulfamic acid, refluxed with an alcohol, produces the corresponding
ammonium alkyl sulfate directly. Sulfamic acid is inexpensive, readily available, and far less hazardous than conc. H2SO4. It's a shame this
isomerization doesn't take place with higher ammonium alkyl sulfates.
PGP Key and corresponding e-mail address
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Theoretic
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The reaction of sulfamic acid with an alcohol gives the alkylammonium hydrogensulfate rather than sulfate:
NH3SO3 + C2H5OH => C2H5NH3HSO4.
A great alternative preparation though. 
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Polverone
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drat
curse my wishful memory
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Mendeleev
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I successfully made some methylamine hcl today using the hexamine method. I did the standard 140 g hexamine reaction. To this I added 320 mL of
water, and then 480 mL of 31.45% HCl. This is basically Rhodium's method to the dot except I adjusted the volume ratios to fit lower
concentration of HCl. The mixture was stirred and refluxed in a beaker for about 1 or 2 hours. There was a white froth or powder at the suface
immediately upon mixing the ingredients. The reflux apparatus was a simple piece of saran wrap, tightened with rubber bands, and full of ice in the
inverted cone, very similar to brainfever's nitric acid distillation apparatus.
After refluxing I proceeded to boil down the liquid until I got down to half of the original volume. The beaker was cooled and a lot of white
precipitate formed, which was filtered. Next the solution was boiled down almost all the way until I noticed a lot more smoke and fish smelling
fumes. After cooling the crystals were one big chunk with almost no liquid in them.
After collecting the crystals, they were dissolved in about 250 mL of boiling ethanol and filtered. There was a lot of precipitate left undissolved,
the ammonium chloride. I will put this to work making more methylamine hcl with formaldehyde. The ethanol was boiled off untill again, there were
lots of fumes and fish smells. Upon cooling the whole mass solidified into a chunk of methylamine with no liquid in it. It is a tad yellowish, but
as I have no chloroform I will simply wash it with very cold ethanol, which I hear also works.
The yield so far, 86 g of recrystallized but not washed mehtylamine hcl. I guess I lost a bit because I boiled down too much and left the
methylamine melt to vaporize for too long, but I am not too worried as this helps me avoid filtering the solution countless times.
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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Organikum
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Use the method with alcohol added, this is faster and avoids dimethylamine formation. (you may have a look at the HIVE for the thread "For the
vindication of Eleusis" for detailed discussion).
Ethylalcohol dissolves a good amount of ammoniumchloride, it is no good solvent for extraction and rarly anhydrous. n-butylalcohol would be best, but
who has? HOT IPA works well and is freely available - anhydrous.
ORG
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Mendeleev
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I repurified my methylamine hcl with cold ethanol, -15 C. I added 100 mL, decanted, then 50, then 40, and then 30. At 30 mL the color of the ethanol
was only slightly tinged yellow. The final yield of pure product was 50 g on the dot. Not very spectacular but its okay. Next time I will add the
ethanol at the beginning as suggested.
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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Jacked
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Reply
How about Methylamine via Nitromethane doing a Al/Hg amalgamation and piping off the Methylamine? Bubbling it through H2O or maybe Alcohol in a flask
sitting on a scale as to calculate saturation amounts? I don't know exactly what I'm talking about but I know this is a method for producing
Methylamine. Actually the Methylamine is a by product of the reaction when it is used with P2P or MDP2P... leave out the drug precursor and you got
it
[Edited on 2-8-2004 by Jacked]
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Mendeleev
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I noticed something strange. I performed the reaction with hexamine and ethanol as Organikum recommended. The first time I added the hcl/ethanol
chilled, the second time not. When the HCl/ethanol was not chilled I noticed a much larger increase in volume during refluxing. In both cases the
reaction was refluxed in a sealed evironement at 60-75 Celsius for two hours before distilling, but the first time the total volume went up from
around 500 mL to 600 mL, whereas the second time it went from 500 mL to 1L. Why is this?
[Edited on 21-8-2004 by Mendeleev]
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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JohnWW
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Partly due to thermal expansion; and another possible reason is that the addition of HCl would have introduced ionic species to the mix, ending up as
[CH3-NH3]+Cl-, which would have attracted fairly large volumes of ethanol molecules to themselves as spheres of solvation, distorting the arrangement
of molecules in the solution.
John W.
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Theoretic
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I suggest oxidative decarboxylation (OXDCO) of acetamide. Hypochlorite would do the trick:
CH3CONH2 + NaClO => CH3NH2 + NaCl + CO2
Acetamide can be made from acetic acid, chalk/soda and any nonvolatile amonium salt:
2CH3COOH + CaCO3 => Ca(CH3COO)2
Ca(CH3COO)2 + (NH4)2SO4 =>
CaSO4 + 2NH4CH3COO =>
CaSO4*2H2O + 2CH3CONH2 (for example).
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Organikum
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Addon to the Zn reduction I posted
For good results additional ammoniumchloride has to be added or some trimethylamine will be formed.
HCl has to be kept on the very low side, iron works too as reducing agent, it requires higher temperatures and more time though.
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Mendeleev
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Does anybody think I could condense methylamine by passing it through a 300 mm graham condenser filled with a 91% solution of IPA at -25 C?
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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neutrino
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I don't see anything wrong with that. Just remember to keep your recieveing container chilled below -6*C.
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Mendeleev
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If you have a substance which is solid at room temperature, but sublimes at a certain different temperature for example, around 150 C, or a solid that
melts at a lower temperature and then vaporizes at 150 C, will that solid sublime if you pull a vacuum strong enough to cause a liquid, which boils at
150 C, to boil at room temperature? I ask this because I have been getting low yields of methylamine using the hexamine, hcl, ethanol method and I
think I may be boiling away a lot of my methylamine when I boil the water. I also recently acquired a very strong vaccum pump.
[Edited on 27-11-2004 by Mendeleev]
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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neutrino
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The liquid boiling doesn’t necessarily mean that the solid will sublime. This depends on the vapor pressure of the substances at whatever
temperature you’re using. To get something to boil/sublime, you have to get the vapor pressure and atmospheric pressure the same. You can do this by
heating the substance (increasing its vapor pressure) or decreasing the pressure around it. If your vacuum pump is a decent one, then should work.
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