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Author: Subject: OTC diethylamine, the easy way
guaguanco
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[*] posted on 28-3-2005 at 14:16


Quote:
Originally posted by garage chemist
Dimethylformamide, a common solvent used in laboratories, could perhaps be split into dimethylamine and sodium formate by boiling with NaOH. Would this work?

Yes.
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[*] posted on 11-4-2005 at 14:17


I mixed a dash of dilute NaOH with a squirt of DMF, the DMF dissolved completely. On heating the solution, a nasty ammoniacal stench was produced.
Of course, DMF is not so easy to get.

What is dimethylamine used for anyways? Why is it listed as a chemical weapon precursor?
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[*] posted on 12-4-2005 at 08:09


DMT synthesis? maybe? not sure exactly. You can also make it by reacting ammonium chloride and paraformaldehyde at high temperatures. It is a byproduct in the production of methylamine.
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[*] posted on 25-9-2005 at 19:45


I have done a few experiments with DEET chemistry today. I added 24% DEET to water, it formed 2 layers, then added IPA till everything went into solution. It ended up a light yellow solution for some strange reason. To this KOH was added(a lot was added) while magnetic stirring until the reaction mixture separated into two layers(both around the same colours, but the top layer a bit darker orange/yellow). The layers were separated with a separatory funnel and to each part (both tested as basic) I added lots of HCl until it was rather acidic. The lower portion upon addition of acid emitted fumes, like the way HCl and ammonia react, and became clear. The upper level upon addition of acid fumed to the same degree as the lower solution, it also became a darker colour, and a white precipitate occured, likely 3-methylbenzoic acid.

I could still smell DEET in both parts, so perhaps refluxing with KOH next time would be benefecial.

Anyone have any ideas on separating the diethyamine from either layer(other than distillation), as a pure liquid or as a diethylammonium salt?



[Edited on 26-9-2005 by rogue chemist]




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[*] posted on 27-9-2005 at 20:40


Sorry about the double post....

I mixed the two solutions together today bacuse I needed one of the flasks for something else, and I was rewarded with a single phase, and a large ammount of precipitate, and the DEET smell was nearly gone. The reaction between DEET and KOH just must require time, but I do not know what chems would be in each initial layer formed, so I do not even know whether the KOH and DEET would have been in the same flask. Although I imagine the KOH and water would have formed one layer, and DEET and alcohols the other layer, which would mean the KOH and DEET could not react as they were in different flasks...Wait I added HCl after...so perhaps just not enough was added to one flask to cause precipitation of 3-methylbenzoic acid.

Oh well, I now have 2 new compounds to lay around my lab in vials, the methylbenzoic acid and after I work up the diethylamine I should get diethylammonium nitrate.
:)




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