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Author: Subject: VX preparation
ANTICIPATE
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[*] posted on 14-7-2008 at 03:43


PATENT NO. IS 3911059,NOT 391059
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Sauron
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[*] posted on 14-7-2008 at 04:17


That is the most important of many patents on this series of compounds because it describes the actual process by which VX, the only one of the series mass produced, was made at the polit plant. Eckhaus, first name on the patent, was director of that plant and codeveloper of the process.

It has been posted on the forum previously.

It would be well to note that the starting material is corrosive and pyrophoric as well as toxic and all the intermediates are potent AChE inhibitors (except for sulfur and ethanol). The only safe way to work with this compound is on paper or on a computer display.




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[*] posted on 14-7-2008 at 04:33


All compounds can be handled safely if you have the right equipment and good technique.

This stuff is pretty nasty but an appropriately set up university lab can handle it with ease.

http://en.wikipedia.org/wiki/Phosphorus_trifluoride
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[*] posted on 14-7-2008 at 05:01


Oh, and phosphorous trifluoride is squitterlingly easy to make if you can get your mitts on some phosphorous trichloride and a suitable metal fluoride.

Mix and stir and it just bubbles off, make sure you have a nice cylinder to condense it in though as it is creeping death :D
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[*] posted on 14-7-2008 at 06:28


There was I time when I thought so as well. There was a time when the people at Edgewood thought so, too, till they found out the hard way to the contrary.

VX is primarily a contact hazard.

HOWEVER it turns out that, even though its vapor pressure at ordinary temperatures is trivial, its toxicity is such that it does present an inhalation hazard at such very low concentrations.

Gone are the days when the EA people worked with VX on open benchtops and in beakers.

We learned a LOT about the effects of low level exposures to these agents in the 80s and 90s and we are still learning and what the shakeout is, is frightening.

So now I must disagree and say: no, a good university lab is not adequate, special precautions are absolutely necessary if you value the integrity of your CNS and those of all others around. It would take a very unusual university lab to be properly equipped to work with this class of military OPA. This isn't Saunders and colleagues at Oxbridge in the 30s and 40s experimenting on each other with DFP. DFP is peppermint chnaaps compared to the V-series.

The Edgewood folks were caught totally off their guard, one of their scientists suddenly had his nervous system go haywire in the middle of the night, at home. Fortunately his wife knew who to call. The man survived but he was never neurologically intact again. Not a pretty sight, I hear. For many years they would trot him in to be shown to classes of new investigators/trainees. It was a very effective demonstration of why it is necessary to take their new protocols seriously, why SCBAs and MOPP gear are mandatory.

VX is persistent and difficult to decontaminate and when you do DC it, some of the degradation and hydrolysis products are still very toxic (though less than VX itself.) Something can be 25X less toxic than VX and still be as toxic as GB and 500 X as toxic as HCN. (OK I pulled those numbers out of my head but they are close enough for argument's sake.)

This why I am unconcerned about discusing this chemistry in the clear: because anyone stupid enough to try it outside of a REAL CW lab, is going to get a lesson in how evolution works. He'll take himself out of the gene pool, permanently. Faster than you can say acetylcholinesterase.




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[*] posted on 14-7-2008 at 06:38


And PS, I would not make the MePF2 from PF3 and methane. That may be a valid industrial process, but in a lab it would suck. MePCl2 is not hard to make, and no great precutions are required if your skills set includes airless operations.

Once you move to the next step, the diester, it's time for moon suits and SCBAs. After that things get steadily riskier.




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[*] posted on 14-7-2008 at 06:44


I am not suggesting handling VX in a university lab.

I am pointing out that PF3 and other such goodies can be handled in a university lab.

I should think that the boys and girls down at Porton Down are set up quite nicely to handle this stuff.

Besides anyone who wants a Darwin Award can always have a go at nickel tetracarbonyl. Contrary to popular belief there are ways of making it apart from the Mond process and one of them starts with stuff you can buy down Walmart :cool:
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[*] posted on 14-7-2008 at 06:48


Quote:
Originally posted by Sauron
And PS, I would not make the MePF2 from PF3 and methane. That may be a valid industrial process, but in a lab it would suck. MePCl2 is not hard to make, and no great precutions are required if your skills set includes airless operations.

Once you move to the next step, the diester, it's time for moon suits and SCBAs. After that things get steadily riskier.


We made PF3 to make metal complexes of the stuff, we had no intention of making MePF2 that way.
We made our MePF2 from MePCl2
Transition metal phosphine chemistry is pretty hot in academic circles.
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[*] posted on 14-7-2008 at 06:55


No problem. We were talking about two different things.



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[*] posted on 14-7-2008 at 07:14


Righto

This was back in the early eighties and there were a few middle Eastern gentlemen working quietly towards their PhD's.

Looking back now with 20 20 hindsight it is quite possible that they were more interested in the phosphine ligands than the metal complexes....
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[*] posted on 14-7-2008 at 08:54


Maybe. Maybe not. The Middle East is a big place, the Islamic world even bigger, and not everyone is motivated in the same way.



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[*] posted on 14-7-2008 at 09:48


Very true and indubitably the case that they would have trained elsewhere if we had not taken them.

But I reckon there are a good few weapons programs around the world that would never have got going without a good technology injection from outside.

http://en.wikipedia.org/wiki/Rihab_Rashid_Taha
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[*] posted on 14-7-2008 at 15:40


Serpent and the Rainbow, A kickass movie. I have not seen it in 14 years. Sauron you got me wanting to see it again, especially since I was fairly young last time I saw it and I did not understand everything going on.



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[*] posted on 14-7-2008 at 17:48




This stuff is extremely nasty, good thing is that all this CW crap now beeing destroyed in US as well as here in Russia.

[Edited on 15-7-2008 by Engager]




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[*] posted on 14-7-2008 at 21:24


In the second to last step, the P=O bond of the "trans-ester" which you drew correctly, is thiated and that compound is then thermally isomerized. The final product however has P=O bond and thioester side chain. You show it with a P=S bond ands thioester side chain.

If you took VX and thiated it you would have the structure you show as final product but that is not VX.




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[*] posted on 15-7-2008 at 00:02


Yes, i just mistyped =) Picture is now corrected.

[Edited on 15-7-2008 by Engager]




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[*] posted on 15-7-2008 at 01:51


There is considerable confusion in what passes for the literature as to the Russian (Soviet era) equivalent of VX also known as Substance 33, which is supposed to be different than the US VX but very similar.

Various books on the subject in the West also talk about VX-x, which may or may not be same as "Russian VX"

Obviously, the confusion is because neither the Russian government nor the US government is willing to state exactly what is what, so information tends to come from anonymous or pseudonymous sources, Cold War era defectors and dissidents, disaffected scientists inside and outside of Russia, and is difficult or impossible to verify. One alleged Soviet V-agent turned out to be a thickened version of GD (soman) and not a V-agent at all.

The situation is even worse as regards the so called novichoks, or nontraditional agents as the West refers to them obliquely.

How much of this could be disinformation is an open question.

I will understand if it would not be convenient for you to comment further.

Thanks for your input above.




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[*] posted on 18-7-2008 at 08:48


Do you think that very low dose atropine ingestion while working with the chemical would immunize him from some of it's nastier effects? Just speculating.

Also, shouldest disposal be a problem due to it being a powerful nerve destroying toxin and all? :o

[Edited on 18-7-2008 by Skrinkle]
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[*] posted on 18-7-2008 at 15:44


The short answer is "No". Atropine is useful with some OPAs but not with VX and never as a prophylaxis.

Disposal? No one here is proposing to make any VX only discussing how in fact it was done by a supposedly sane and responsible government. They are the ones with the disposal problem.

There is an excellent book in References on the chemistry, toxicology, therapeutics and pharmacology of chemical warfare agents. I recommend it.agents.




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