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jimwig
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[*] posted on 9-6-2008 at 14:25
VX preparation


follows: the patent description of preparaation of nerve (war) gas

Description of US391059



This invention relates to the manufacture of S-(2-dialkylaminoethyl) O-alkyl alkylphosphonothiolates. These compounds have the formula ##EQU6## wherein R, R@1 and R@2 are lower alkyl groups. R is preferably methyl or ethyl, R@1 is preferably methyl, ethyl, isopropyl, n-propyl or butyl, and R@2 is preferably methyl, ethyl or isopropyl. Of all the compounds, S-(2-diisopropylaminoethyl) O-ethyl methylphosphonothiolate is regarded as the most important. The compounds have extremely high percutaneous toxicity to mammals and are useful as chemical warfare agents.

Our method involves the addition of sulfur to a 2-dialkylaminoethyl alkyl alkylphosphonite of the formula ##EQU7## giving an O - (2-dialkylaminoethyl)-O - alkyl alkylphosphonothioate of the formula ##EQU8## which is isomerized by heating to give our desired compounds.

We have found that if certain precautions are taken it is possible to secure consistent yields, in the range 95-98% of the theoretical, in the sulfur isomerization steps and the product is of such purity that no subsequent purification step is required.


this is only the first few paragraphs. i am interested in not only this most dangerous gas from a preparational point of view but also a historical one. the federal of american scientists talks about this a bit on its site.

and also there is the "missing wma" from iraq and hussein's/bush's era of ?????

i have read but cannot find a description of the extreme conditions of saafety employed to manufacture this gas. that also included some words about onsite accidents aand their outcome.

any interest?

[Edited on 9-6-2008 by jimwig]




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[*] posted on 9-6-2008 at 15:41


Why people want to prepare war gasses for the sake of preparing a chemical warfare is beyond me.



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[*] posted on 9-6-2008 at 15:46


Indeed even explosives can be used to help people and save lives. But I can't say the same for nerve gas why would you want it?



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[*] posted on 9-6-2008 at 16:34


Wait a minute now, nerve gas has legitimate uses. Maybe he just wants a really, really, really effective pesticide?
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[*] posted on 9-6-2008 at 17:02


A human pesticide?
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[*] posted on 9-6-2008 at 19:05


First of all the US and UK patents relating to VX and other V-agents have been posted here before.

Secondly, anyone who tries to actually make this will be dead faster than you can say acetylcholinesterase.

Aum Shin Rikkyo spent $11 Million US on their lab to prepare GB and VX and still had a number of accidents.

The intermediates and precursors to V-agents are also quite toxic, more than enough to be lethal under ordinary conditions, and so a wannabe VX maker will be dead long before he gets to the end product.

There is nothing wrong with studying this technology. There are indeed insecticides closely related to VX, that have been useful to mankind. One such is actually mentioned in the CWC - that's how close it is.

A number of OPAs do find use in medical research.

So study, ywes, if one is interested. Understand, yes. Prepare, NO. Not unless you have a world class deathwish.




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[*] posted on 10-6-2008 at 04:12


Quote:
Secondly, anyone who tries to actually make this will be dead faster than you can say acetylcholinesterase.


Hilarious :D




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[*] posted on 10-6-2008 at 04:23


I dont know whats the point of studying such things as you can never do them. If its a way of commiting suicide one is after VX is a very longwinded way to go and theres always the chance of failure - maybe its the not knowing that makes it interesting.
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[*] posted on 10-6-2008 at 06:59


Now this is a darn- funny thread!

Jimwig: Download or rent this movie: The Rock (With Nicholas Cage and Sean Connery)

Ask yourself again if you really want to make this nerve- agent...




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[*] posted on 10-6-2008 at 07:02


All the G agents and V-agents were originally developed as insecticides. Sarin, Soman and tabun in the 30s by Schrader at Baeyer IIRC. The V-agents in the 1950s initially in the UK.

All are relatively simple OP molecules, and if one is at all interested in OP, it is well worth knowing in some details what NOT to build, or one can get in a lot of trouble, in more ways than one, quite by accident.

The Baeyer people simply found that certain strucures unexpectedly possessed very high mammalian toxicity and in the process learned how to turn that toxicity on and off, as it were. In other words, knowing how to make insecticides that are effective while possessing low mammalian toxicity is inseperable from knowing how to engineer high mammalian toxicity.

Things like parathion and malathion are not very far away from either class of military agent.

The V-agents were "improvements" possessing extremely high percutaneous toxicity against mammals, including man.

Again, there are commercial insecticides that are in the same general class, they just don't have the specific molecular features that optimize certain effects for military purposes.

These are first and second generation OPAs we are talking about. There are at least four or five generations out there, the governments have simply gotten somewhat better at keeping a lid on most of that (but not all.)

Unless one knows the chemistry and SARs of these things, how can one even begin to think about decontamination, prophylaxix, therapy, design or detection equipment or protective apparel and equipment?

Pharmacologists and medicinal chemists are always intensely interested in anything possessing extremely potent biological effects. That's why the natural toxins like saxitoxin, from red-tide infected shellfish, or the fugu toxin (also employed in zombie dust) are interesting to those disciplines. (Tetradotoxin). See The Serpent and the Rainbow sometime.

Even the mustards, scourge of WWI, eventually produced pharmacological windfalls of great benefit to mankind. Cancer chemotherapy would not exist without them.

This is simply knowledge. How knowledge is used is entirely dependent on human beings. There's no such thing as evil knowledge, just evil applications of that knowledge. There is nothing mankind was not meant to know. Lines like that belong only in B-grade sci fi movies.

Anyway, everything I know about this subject came from the open literature and surely none of that is off limits here.




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[*] posted on 10-6-2008 at 07:05


BTW ScienceGeek, that film had almost NOTHING to do with reality as far as VX was concerned. Hollywood bullshit. A bad place to get one's chemistry.

VX is low volatility, kills almost exclusively by contact with the skin, so all that garbage about the marine dropping the little globe and then having his skin melt off, was horseshit.

Some Hollywood asshole decided that would be more impressive visually than just having him to the dance that we used to call "Deadbug" in the military, where you get on your back end emulate a cockroach sprayed with RAID.

That's what it does. It's an enzyme inhibitor,

The G-agents are volatile, but VX used to be worked with on the open desktop till the Edgewood people found out the hard way that there was a chronic low level exposure problem. Now it's in the hood, too. They used to trot out one of their scientists who had his nervous system profoundly affected by working with VX on the benchtop too long, to impress new personnel with the need for the containment procedures. He was not a pretty sight.

No I never worked there but I have friends who did. And I have been there.

[Edited on 10-6-2008 by Sauron]




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[*] posted on 10-6-2008 at 10:06


most infatically not interested in preparing --- just the preparation. process is my interest - not necesarily product......

thanks Sauron for the memory boost - as i mentioned i have forgotten the historical aspect of this whole topic. i for some reason just wanted to regain my recollections.

and of course the personal knowledge of the plants involved......!!!

the lecture i knew would be given so thanks anyway.....

many many procedures, protocols, etc are discussed here. i enjoy most all of them and sincerely apprreciaate the opportunity to learn even in a small manner.

having said that i aalso would argue that very few of those things presented here onl this board reach any sort of production stage -- despite what may be said. i could be wrong......

so it goes




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[*] posted on 10-6-2008 at 12:59


I've seen the Rock recently, and highly doubt the skin melts off. It's hollywood bunk. You can also read the MSDS on VX here. Though it would make sense to mix it with a dye, in case of a leak, the green color is also added for special effects, as VX is colorless to straw colored.

The volatility at 25ºC of the common nerve agents is here from Kirk-Othmer "Chemicals in war":

GA: 610 mg/m3
GB: 21,900 mg/m3
GD: 3,060 mg/m3
VX: 10.5 mg/m3

From this list I would say not VX is the most frightening, but GB. The volatility of water at the same temperature has been said to be 23,000 mg/m3. More on toxicological data from the Federation of American Scientists, estimates for 70 kg man:

...Route ....................................................Form........Effect.....Type ......GA .........GB........GD.........VX.........Dosage
Inhalation at RMV = 15 liters/min..........Vapor......Death.....LCt50.....135.........70..........70..........30..........mg•min/m3
Percutaneous.....................................Liquid......Death......LD50.....4,000.......1,700.....350.........10...........mg

The volume of a drop is something like 0.02 mL, so if 10 mg percutaneous is deadly for VX (70 kg man), then since v = m/d: 0.01g/1.0083g/cc = 0.01 mL, so about half of a drop is deadly 50% of the time. Though by a subcutaneous route, it will likley require much less, probably in the microgram range.

[Edited on 10-6-2008 by Schockwave]
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[*] posted on 10-6-2008 at 15:42


So that means sarin spills are the most dangerous, followed by soman.
However, AFAIK, VX attacks will be done by creating a mist of VX in the battlefield (very small droplets). Not sure, though.
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[*] posted on 10-6-2008 at 17:01


Yeah, the deadliest common one per raw chemical handeling basis I would say is GB. It is much easier to avoid skin contact than inhalation. However, dispersed in specialized aerosols, specifically engineered bombs, etc. VX is the worst.
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[*] posted on 10-6-2008 at 17:32


Please note that while the chemistry of these comounds is fair game on this forum, my understanding is that the weapons engineering of them is definitely out of bounds.



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[*] posted on 10-6-2008 at 19:54


To weaponize them requires far more complex procedures than a simple discussion.
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[*] posted on 10-6-2008 at 22:23


True, but the forum proprietor demands no such discussions at all. Not chemical weapons (as opposed to the chemistry involved), not explosive devices (as opposed to the chemistry of energetic materials) and so on. I agree with him.

Just a cautionary reminder. I'd hate to see the thread get Detritused or locked because someone runs his mouth the wrong way.




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[*] posted on 12-6-2008 at 10:01


Quote:

dont know whats the point of studying such things as you can never do them.


Why study drugs?
Why study nuclear weapon design?
Why study other galaxies?
Why study anything that you can't or probably won't "do"?

Knowledge.

I'll probably never go to Siberia, never time travel, go to the moon, go to Egypt or synthesize F2, Me2Hg or cocaine but I still choose to study them. Why? Knowledge is power. Knowledge is fun. It's just the "beezneez".

Studying chemical weapon manufacture is no different than studying how fission is induced in plutonium. To each his own. I think people who study anything should be praised.




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[*] posted on 12-6-2008 at 14:29


Quote:
Originally posted by MagicJigPipe
Quote:

dont know whats the point of studying such things as you can never do them.


Why study drugs?
Why study nuclear weapon design?
Why study other galaxies?
Why study anything that you can't or probably won't "do"?

Knowledge.

I'll probably never go to Siberia, never time travel, go to the moon, go to Egypt or synthesize F2, Me2Hg or cocaine but I still choose to study them. Why? Knowledge is power. Knowledge is fun. It's just the "beezneez".

Studying chemical weapon manufacture is no different than studying how fission is induced in plutonium. To each his own. I think people who study anything should be praised.


Well I would like to go to Siberia and time travel or go to other galaxies but I don't want to make VX gas. Even with a top of the line lab and millions of safety precautions I don't want to make it. For starters the synthesis isn't interesting and the products only purpose is to kill.


Even studing radiation can benefit mankind with irradiating food, microwaves, atomic clocks and nuclear power plants. Cocaine in correct doses CAN be used to relive pain or aid other problems. VX gas has been studied extensively and has the sole purpose to kill.




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[*] posted on 12-6-2008 at 18:13


Who says this synthesis is not interesting? Whoever says that does not understand the synthesis or the precursors involved.

Who says the only purpose of chemical weapons is to kill? That's a sophomoric simplification. There have been many serendipitous discoveries that sprang out of CW research. I have stated many of them before so I do not feel called upon to state them again just to refute such a childish remark.




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[*] posted on 12-6-2008 at 19:11


We have closed threads for ideological bickering before, but that need not happen to this thread, further posts not chemistry related will be removed. Chemistry discussion of CW agents are just fine.



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[*] posted on 12-6-2008 at 21:24


The starting material, methyldichlorophosphine, MePCl2, is not commercially available AFAIK, and is not easy to prepare. It is very air and moisture sensitive and is pyrophoric. It is also toxic. I have posted about its preparation previously. Making it would be rather technique-intensive.

The type and quality of sulfur employed is critical.

The esterification and transesyerification steps are equilibrium controlled. Isolation of the desired product by fractionation is necessary.

The nitrogenous side chain is recognizably a close derivatibe of Hunig's base, the famous non-nucleophilic strongly basic tertiary amine. The properties of this side chain, its steric hindrance, and the S-CH2-CH2-NR2 structure all point to the liphophilicity and persistance.

The thermal isomerization is the last step.

All of the precursors and intermediates are toxic. The final product is extremely so.

While I would not care to conduct this preparation, I certainly regard it as interesting organophosphorus chemistry.




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[*] posted on 13-6-2008 at 20:52


I suppose from Di-isopropylamineethylchloride hydrochloride it wouldn't be too far a stretch to make the S substituted compound?



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[*] posted on 13-6-2008 at 21:41


You would not have to make the thiol.

You make the aminoethanol. transesterify that with the diethyl ester of the methylthiophosphonate, (itself made from the dichloride). Purify that to obtain the mixed ester that is desired, and then you are ready for the thermal isomerization.

The P=S sulfur exchanges with the O of the aminoethyl ester and voila. Read the patent posted by thread author and the related UK patents I posted last year. It's all there in the open lit.

Of course they don't tell you how to survive the synthesis. For that you have to more or less take a job at Edgewood, or Porton Down, or some similar facility of the sort, still allowed under CWC.

I first saw that patent about 27 years ago.




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