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guaguanco
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In the real world, intermediates like O,ethyl dichloro phosphonate are prepared from POCl3 via fractional distallation. Lacking than it's well
nigh impossible to prepare a pure ester like that.
It's not hard to replace the chorine atoms with fluorine atoms in a suitable aprotic solvent. Again, this reation is pretty much out of reach of
the home experimenter working with beakers in the garage. The resulting fluoro-esters get so toxic so fast that you just can't risk *any*
exposure to them.
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DDTea
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Oh, you present too much reason/fear of the unknown for us mad scientists, guaguanco. We're all about doing the impossible, or the next to
impossible, or just what is crazy and wild and immediately harmful to life and limb  .
You are right on the question of Fluorinating POCl3. The reaction requires Antimony Trifluoride and Hydrofluoric Acid, and some mildly complicated
apparatus. But it's not impossible by any means. There are always alternative methods (ahh, the mad scientist optimism).
Why would you need O,Ethyl Dichlorophosphate in the production of Tabun? It is much easier to add the Ethyl and -CN groups in the last stage of the
synthesis. N,N-Dimethyl Dichlorophosphate is reacted with NaCN in Ethanol, and the product is Tabun. Details such as temperatures and pressures can be
worked out later; but at the moment we're hoping to get the groundworks-- notably, POCl3.
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DDTea
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Here's something interesting, from the Federation of American Scientists (www.fas.org)... I grabbed the excerpt from http://www.panix.com/~hncl/HectorsJournal/archives/000109.ht... :
| Quote: | | Tabun synthesis does not require the use of corrosive starting materials and does not produce highly reactive intermediates. The two-step process
involves mixing the ingredients and a carrier solvent in a reaction vessel equipped with a sodium-hydroxide scrubbing system to neutralize the gaseous
hydrochloric acid (HCl) byproduct. A relatively simple air-tight enclosure is also needed to prevent the escape of toxic vapors. The ingredients must
be added in the correct order, without heating, and the vessel cooled to keep the reaction from building up too much heat. Little or no distillation
equipment is required, although the purity of tabun can be increased to more than 80 percent by removing the carrier solvent and the off-gasses by
vacuum distillation. In sum, tabun production is relatively easy because it does not include the difficult alkylation reaction needed to make the
other nerve agents. The major technical hurdle in tabun synthesis is the cyanation reaction (in which a cyanide group is added to the central
phosphorus), because of the difficulty of containing the toxic hydrogen cyanide HCN gas used as the reagent.. |
Why would HCN be needed? Most synthesis sources I've seen say that NaCN is fine. Then again, some Sarin sources say HF can be used in
fluorination, while others recommend NaF. I suppose either way can work...naturally, the amateur would choose NaCN to address the issue of handling.
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guaguanco
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| Quote: | Originally posted by Samosa
Oh, you present too much reason/fear of the unknown for us mad scientists, guaguanco.
You are right on the question of Fluorinating POCl3. The reaction requires Antimony Trifluoride and Hydrofluoric Acid, and some mildly complicated
apparatus. But it's not impossible by any means. There are always alternative methods (ahh, the mad scientist optimism).
Why would you need O,Ethyl Dichlorophosphate in the production of Tabun? It is much easier to add the Ethyl and -CN groups in the last stage of the
synthesis. N,N-Dimethyl Dichlorophosphate is reacted with NaCN in Ethanol, and the product is Tabun. Details such as temperatures and pressures can be
worked out later; but at the moment we're hoping to get the groundworks-- notably, POCl3. |
Well, just call me the little BlueBird of pessimism... 
I was referring in general the the mono-substitution of things onto POCl3. It's very hard to just stick on one (CH3)2N- group and get a pure
product. But knock yourself out!
(Actually, if you really did these reactions in your garage you'd probably end up doing a lot more than knocking yourself out.  )
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chloric1
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POCl3
I remember reading that P2O5 could be heated with anhydrous FeCl3 for POCl3. Would not know a what temperature. Wanting to try.
Fellow molecular manipulator
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Sarevok
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Tabun is made by reacting dimethylamidophosphoryl chloride with sodium/potassium cyanide, and ethanol. Details can be found at DE767511 and DE767830*
(search for it on esp@cenet).
Dimethylamidophosphoryl chloride is made from dimethylamine and phosphoryl chloride. Details can be found at GB744484.
Dimethylamine can be made by neutralizing dimethylamine hydrochloride with alkali hydroxide, followed by the separation of the amine by distillation.
Dimethylamine hydrochloride can be made from ammonium chloride and formaldehyde - see Vogel's A Textbook of Practical Organic Chemistry,
including qualitative organic analysis, pages 415-6.
Phosphoryl chloride can be made from any phosphoric acid, activated carbon, and chloride (or chlorine and carbon monoxide), or from any phosphoric
acid and phosgene (which can be made by oxidizing chlorform (made from acetone and bleach)), etc. See details at GB416084, GB336065, US2622965,
US2712494, US1381783, GB727950, US1462732, GB617990, US2002277, US1921370, US2712494, and GB617990.
Sodium or potassium cyanide were made from urea, carbon, and alkali hydrogen carbonate, by Mr Cool (of rogue science) and Polverone.
*: This patent was found by teshilo, of the rogue science forum. The other patents were found by myself.
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Mendeleev
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This is interesting that most of these G-agents are synthesized from phosphorus oxychloride as opposed to phosphorus tri and penta chlorides. Could
anyone detail a procedure from the tri or penta chloride? These would be easier for me to synthesize than the oxychloride.
Edit: Oops, should've searched google more carefully. Megalomania has an awesome synthesis for damn near OTC sarin. Here's the link http://www.roguesci.org/archive/1043_6-27.html However I missed the part where he went from phosphite to phosphonate, was it when the methyl
iodide adds the methyl group and one of the isopropyls falls off? Does the oxygen that was on that isopropyl become double bonded? Seriously though
that is so damn near OTC it's scary. In a good way of course .
Edit2: I am not sure how to convert this to tabun synthesis. I suppose in the place of all the isopropyl groups, you would ethanolize the hell out
of it, but then you need to attach the dimethylamine, which poses a problem in that the methyl group in the sarin synthesis was added because it was
methyl iodine, but I have never heard of halide amines. (Edit3)Well there is nitrogen triodide, but I would not put this stuff in a flask with G
agents. This step would be even more important because I think it is the part where the oxygen becomes double bonded creating the phosphonate. But
I guess the nitrile group could be added in the same manner as the fluorine atom in sarin, by using carbonyl chloride and then refluxing in ether with
sodium cyanide.
[Edited on 13-7-2004 by Mendeleev]
[Edited on 13-7-2004 by Mendeleev]
[Edited on 13-7-2004 by Mendeleev]
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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DDTea
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One way of attaching a Cyanide group on Organic Phosphate compounds is through Cyanogen Iodide... I just know the reaction, but not the method to do
it. From Phosphorus Pentachloride, Phosphorus Oxychloride can easily be made by simply adding water.
Trying to produce Tabun via megalomania's route, or something similar, would be a very round-about and difficult way... I say stick with the
Dimethylaminoethylphosphoryl chloride route.
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Texium
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Thread Pruned
15-6-2017 at 17:47 |
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