Sciencemadness Discussion Board

Methylamine HCl with a pipe bomb

phendrol - 15-6-2012 at 03:33

Hello

I'm thinking about preparing methylamine hcl with a pipe bomb. I made it some time ago from hexamine with much success, but the pipe bomb route seems to be even less labour intensive. The only thing that discourages me, is that there are chances of a serious accident while attempting the synthesis.

The recipe is as follows:

400 ml of methyl alcohol with 535 grams of ammonium chloride, 400 ml of water, and 2.5 grams of ferric chloride are heated in a 2 l pipe bomb to 300 C for two hours.

Now could anyone give me a clue on the pressure inside the vessel? Will a steel pipe, with 2mm thick walls survive it?

haroldramis - 15-6-2012 at 04:45

reference please?

hyfalcon - 15-6-2012 at 08:46

I wouldn't want to be around it. Just water alone superheated can generate quiet a force in and of itself. If you were standing in the wrong spot when it failed, well, it wouldn't be good.

chemrox - 15-6-2012 at 11:06

If hexamine was too much hassle I wonder about making the pipe bomb. Surely you wouldn't just hop down to the plumbers supply and buy galvanized steel parts?

bbartlog - 15-6-2012 at 12:22

Vapor pressure of methanol at 300C is about 2000 psi. Whether a pipe with 2mm thick walls would survive it depends on the type of steel and the diameter of the pipe, among other things; in general I would worry more about failure at the ends/caps/flanges. And I would recommend the Hofmann degradation of acetamide as a less dangerous and more easily controlled method of synthesis.

phendrol - 15-6-2012 at 23:59

It's taken from US patent 2085785. I think I will try it in about a week or two. You can be sure I'll post my results.

turd - 16-6-2012 at 13:37

Quote: Originally posted by phendrol  

400 ml of methyl alcohol with 535 grams of ammonium chloride, 400 ml of water, and 2.5 grams of ferric chloride are heated in a 2 l pipe bomb to 300 C for two hours.

Now could anyone give me a clue on the pressure inside the vessel? Will a steel pipe, with 2mm thick walls survive it?

:o Are you completely out of your mind? Switch to theoretical chemistry, at least you won't hurt yourself/others.

haroldramis - 16-6-2012 at 16:34

Thanks for the info on that Patent. Out of all the amine making documents Ive seen, i never saw that one before. Looks like quite a gem if it works as advertised.

Ill be anxiously awaiting your results.

...

ItsAChitzen - 18-6-2012 at 10:35

Wtf? There are better ways to make this. Also, it is cheap as fuck. Also, it is a Precursor. You know the one I mean. LoL to you and those helping you...

chemrox - 18-6-2012 at 22:42

Quote: Originally posted by phendrol  
It's taken from US patent 2085785. I think I will try it in about a week or two. You can be sure I'll post my results.


This patent number yielded something called "Tag Package" What is the correct number?

phendrol - 18-6-2012 at 22:54

Quote:
Wtf? There are better ways to make this. Also, it is cheap as fuck. Also, it is a Precursor. You know the one I mean. LoL to you and those helping you...


It's not a controlled substance where I live, and if you know better ways to make this, please share...
Quote:
This patent number yielded something called "Tag Package" What is the correct number?


http://www.freepatentsonline.com/2085785.pdf

ItsAChitzen - 19-6-2012 at 09:44

Quote: Originally posted by phendrol  

It's not a controlled substance where I live, and if you know better ways to make this, please share...



If it isn't a controlled substance, I would buy it from a manufacturer...

[Edited on 19-6-2012 by ItsAChitzen]

madcedar - 19-6-2012 at 13:47

Since nothing interesting comes up when using the sciencemadness search engine, I think you'll find the links below useful.

Acetamide to Methylamine
http://www.sciencemadness.org/talk/viewthread.php?tid=7410

Good way to Methylamine HCl?
http://www.sciencemadness.org/talk/viewthread.php?tid=1261

Methylamine Purification
http://www.sciencemadness.org/talk/viewthread.php?tid=9139

Cheers

PS: Oh by the way, the main problem with using the bomb is that (from reading between the lines in the patent) it seems the major product of the reaction will be the diamine and not the mono-amine you are after.

[Edited on 19-6-2012 by madcedar]

turd - 20-6-2012 at 00:36

No, the main problem with "using the bomb" is that it has an appreciable chance of killing or seriously hurting him. If you lack the equipment and experience, then you don't do high pressure reactions. Period. Aside from the economic stupidity - for the price of a real autoclave you can buy MeNH2.HCl lasting more than a lifetime.

madcedar - 20-6-2012 at 15:20

Quote: Originally posted by turd  
No, the main problem with "using the bomb" is that it has an appreciable chance of killing or seriously hurting him. If you lack the equipment and experience, then you don't do high pressure reactions. Period. Aside from the economic stupidity - for the price of a real autoclave you can buy MeNH2.HCl lasting more than a lifetime.


100% correct.

One more reference for you Phendrol that seems easy and safe:
http://www.erowid.org/archive/rhodium/chemistry/methylamine....

AndersHoveland - 21-6-2012 at 02:58

I would also like to mention another similar "pipe bomb" reaction; one that could be used to convert urea into guanidine:

By heating urea, ammonium chloride, and aluminum sulfate together with ammonia under pressure, guanidine can be obtained. The reaction products are boiled with an ammonium hydroxide solution to precipitate out the aluminum hydroxide. The remaining clear filtrate contains guanidine hydrochloride, ammonium sulfate, unreacted urea, and unreacted ammonium chloride. Using equimolar ammounts of NH4Cl and urea, with one third of a mole aluminum sulfate for every mole of urea, heated to 275degC, and subjected to 6.8 atmospheres of pressure, the yield of guanidine (relative to initial urea) was 28% after 30 minutes, and 34% after two hours. Using excess NH4Cl increased the yields further.



BooMMaker - 14-8-2012 at 05:41

HMTD isn't a bad choice either, if you want to stick with hex.

SM2 - 14-8-2012 at 06:14

Well, my personal favorite, is to reduce nitromethane in an acidic (HCLaq) environment using activated aluminum. Clean up your almost pure white xtals of methyl-ammonium chloride. If you need Ethylamine HCL, just use Remove, artificial nail remover by Gena labs.

#maverick# - 18-8-2012 at 02:49

Interesting concept, but as others have said, dangerous, stupid and there are easier ways, ive personally made methylamine using this method http://www.sciencemadness.org/talk/viewthread.php?tid=7410


[Edited on 18-8-2012 by #maverick#]

unionised - 19-8-2012 at 01:45

Am I the only one who thought
NH4Cl ---> NH3 +HCl
Fe + 2HCl --> FeCl2 + H2

And
2 FeCl3 + Fe ---> 3 FeCl2

So there's less metal holding the pressure and more gas (the hydrogen) exerting that pressure.
This doesn't seem a good idea to me.

S.C. Wack - 19-8-2012 at 16:49

Glass bombs and ZnCl2 were tried first here:
http://www.sciencemadness.org/talk/viewthread.php?tid=1261&a...
"they failed"

zed - 29-8-2012 at 14:15

The conditions initially proposed would probably require the use of a Parr-type high pressure reactor. If you don't have one, small diameter stainless steel tubing can withstand very high pressures.

We have had similar discussions on producing Diethylamine by such procedures. Except that, ammonium acetate is used is used as a starting material, rather than ammonium chloride. My intuition is, that ammonium acetate might be less corrosive.

beatle_guce - 16-10-2012 at 18:33

just use one of those high pressure co2 tanks for paint ball. I think they have ones thats good for 3000-4000psi youll have to expel all the gas first then muscle a monkey wrench to open it up, then clean out the interior, load it up and close

UnclearReactor - 19-10-2012 at 08:58

The paintball tank is NOT rated at 300° C. It's much weaker when that hot. The aluminum it is made of will react and corrode (but so would the zinc on a galvanized pipe, the iron in a black Iron pipe, not to mention contaminating the reaction). This is a recipe for disaster.

methylamine synth

Mildronate - 20-4-2013 at 10:38

I read in Festers Advanced Techniques of Clandestine Psychedelic & Amphetamine Manufacture book, methylamine synth from MeOH and NH4Cl in high preasure, does it really work?


Attachment: metila.pdf (1.6MB)
This file has been downloaded 5842 times

zed - 20-4-2013 at 15:13

Well, yeah....it might. Such a technique is purported to work, when applied to Formamide or Acetamide. But keep in mind, in those cases, it requires a lot heat, a lot of pressure, and after hydrolysis... and a mixture of primary, and secondary, amines is recovered.

So, is this techniques really better than others?

I don't know. I wouldn't do it. There are easier, and safer ways.

Might be a worthwhile method for producing producing Diethylamine, however.

[Edited on 20-4-2013 by zed]

Mildronate - 20-4-2013 at 23:54

I dont do it this way, but its interesting.

Fantasma4500 - 22-4-2013 at 11:16

just cap it off with aluminium foil at the top. problem solved (:
sounds interesting, i have considered using a pipe of pipebomb type with such endcaps a few times aswell and i have located a piece perfect for the purpose.. perhaps calcium acetate into acetone?

hafnium - 22-4-2013 at 11:45

Perhaps I'm off base here, but isn't preparing methylamine with formaldehyde and ammonium chloride the normal procedure?

"In the laboratory, methylamine hydrochloride is readily prepared by treating formaldehyde with ammonium chloride.[3]
NH4Cl + H2CO → [CH2=NH2]Cl + H2O
[CH2=NH2]Cl + H2CO + H2O → [CH3NH3]Cl + HCOOH"

hafnium - 22-4-2013 at 11:48

I'm also at a loss as to why you decided to post this in the reagents and apparatus section, this should be moved to somewhere else.