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Iv4
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Tabun-think I got it
Dimethylphoprylcyanide/Tabun.I been thinking about this for a while no and I thnk I got it's synthesis down.This is the first time I've ever
tried to come up with the synthesis and my chemistry skills are'nt too good,so be please be gentle 
I'm thinking dimethylamine could be used as the starting point.With caclium phospahte I'm thinking/hoping for demethylphospate.Or would this
require phophoric acid?After that I think cyanogen iodide could place the cyanide bit in.Maybe hcn on the calciumphosphate itself?
The other way (this I havent really thought over but just a thought).Hydrogen cyanide on calcium phosphate and then in methanol.I'm hoping to
have calcium hydroxide and a cyanide/phospouros 'thing'(lack of better word-told you my chemistry is shit).Then if that could be added to
methanol I'm thinking I might get methylphoprylcyanide(not the same but thinking that it could be similer).
[Edited on 5-8-2003 by Iv4]
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DDTea
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Well, we all have our firsts, and our firsts tend not to be our bests 
First and foremost, you don't seem to have Tabun's structure right. Tabun is N,N-Dimethyl O-ethyl Phosphoryl Cyanide (I hope I got the
nomenclature right, because I never quite got it down for Phosphates...). Dimethyl Phosphorylcyanide is another OP, which may or may not have high
toxicity (I have never looked into it- but Organophosphates w/ a reactive leaving group such as -CN, -F, -Cl, etc. tend to have high toxicity).
The purpose of Dimethylamine is not to form Dimethyl Phosphate, but rather get the N,N-Dimethyl group attached directly to the Phosphorus. This is
the tricky part, and I don't believe such a between Dimethylamine and Phosphoric Acid would give you what you want (if it reacts at all).
That is why in the Tabun synthesis, they prefer to use Phosphorus Oxychloride- because the Chlorine is attached directly to the Phosphorus atom, and
does not like to be there . As such, it is reactive and gives the desired results.
So then you bring in the Dimethylamine, which reacts w/ the POCl3, and forms N,N-Dimethyl Phosphorus-Chlorine crap (as I said, I never quite got the
nomenclature  ) and HCl.
To get the O-Ethyl group onto the phosphorus, The N,N-Dimethyl Phosphorus crap is reacted with Ethanol is used- which forms more HCl as the side
product.
Finally, Sodium Cyanide is reacted, and Sodium Chloride is the side product.
As far as the Calcium Phosphate goes, I think you'd be better off working with straight Phosphoric Acid...but still, don't expect wonderful
results from that either.
Better choices may include Phosphorous Acid or Phosphine (some things which I am looking into, but haven't found much time to do serious
research on).
Perhaps you could react N-chlorodimethylamine with Phosphorous Acid, thus attaching the Dimethylamine to the Phosphorus, then react the product with
Ethanol to attach the Ethyl group. The trouble after that, though, is attaching the -CN group directly to the Phosphorus  .
But keep in mind- this is just random stuff I've thought up in a hurry; it probably won't work...just something to keep you thinking .
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DDTea
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Now that I think about it... If you are still interested in Dimethyl Cyanophosphonate...
Perhaps you could react Cyanogen Iodide with the Phosphorous Acid, and then react the product with an excess of Dimethyl Sulfate?
Alternately, if you're looking to be nasty, perhaps a current of straight Chlorine might displace the non-acidic Hydrogen in Phosphorous Acid?
From there, I imagine you could react that with HF, KF, or NaF to get the corresponding Flouride...
Does this sound like a different way to DFP? Or am I just spewing chemical-diarrhea again
BTW- Tabun's PROPER nomenclature is "O-Ethyl N,N-Dimethyl Phosphoroamidocyanidate."
Also, does anyone have much information related to Hexafluorophosphoric Acid? Such as, what is it used in, and any regulations?
I'm interested in if it can be converted to Phosphorus Oxyfluoride .
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Iv4
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Thanks
Thanks for the reply.Fraid I dont have anything to offer back.
Phosphine is used for rat killing in some remote places still so I'll see if I can get some and sneak it into the UK before my flight(and
ofcourse there's the ugly kid to check potency).Is this my trip talking(really need to be more carefull from now on-not the most encouraging
thought for anyone in london?)or is phospouros acid used as a rust remover?
PS
Come to think of it (from a warfare prespective)wouldnt VX pose itself better?
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DDTea
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All the different Nerve Agents have their specific uses on the battlefield; some do certain jobs far better than others. VX is an area-denial weapon,
while Sarin is a quick-gas weapon (due to its fast action), and Tabun fits somewhere in between.
I don't know about Phosphine, however. I believe the Hypophosphoric and Metaphosphoric Acids would be much better options.
Now, in regards to how to purchase said acids... I have read that Metaphosphoric Acid (aka Phosphorous Acid) is used in some limescale removers in
Pool Stores and such... However, it is mixed with a few other acids too
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Iv4
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I supose that very true.What I meant is that with the effort to make 100mls of tabun you could get 40 mls of VX for example.
PS
I'll be looking for diferent acids.
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DDTea
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Looking at this thread makes me recall a discussion with Vulture a few weeks ago. We were discussing the synthesis of Phosphorus Oxychloride from
Phosphoric Acid or Phosphorus Pentoxide.
Basically, Carbonyl Chloride reacts with them at high temperature (around 500*C) to produce Phosphorus Oxychloride. Carbonyl Chloride can be
substituted by straight Carbon Monoxide and Chlorine gas. Similarly, Phosphoric Acid can be a substitute for Phosphorus Pentoxide, but the reaction
seems so much cleaner using P2O5 and COCl2.
After getting Phosphorus Oxychloride, we all generally know what to with it
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Iv4
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But since carbon monoxyde and phosphoric acid are cheaper it would be better right?Since that way you could make up for th ineficiancyby working in
larger amounts.
I'm thinking something like a methbomb?
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Wolfram
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Oh please...!!!!
What normal person would be interested in manufacturing tabun in the garage for personal some needs.
It is not that he is trying to make home made firecrackers..
Obviously this person is´nt connected to any department since he writes: "my chemistry skills are'nt too good,so be please be gentle"
I hope I dont live near where you live.
[Edited on 13-10-2003 by Wolfram]
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Haggis
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Many home scientists produce such chemicals for just the pure satisfaction of doing it. I, for one, am a person to make something, write up in my
little notebook about it, store it in a vial or similar on my shelf and forget about it. I keep it till I either get sick of it (sometimes literally)
or need the container. Others like to have knowledge of such things, which is most likely the case. These 'knowledge junkies' enjoy
knowing all sorts of 'bad' information just because they can. Just because one speaks of such things does not mean they have the intent to
manufacture said chemical, or even use said chemical.
Edit: Take a look around, we aren't 'normal people'.
[Edited on 13-10-2003 by Haggis]
Great ideas often receive violent opposition from mediocre minds.
<b> <a href=\"http://pgp.mit.edu:11371/pks/lookup?op=get&search=0xEE41A2B1\">PGP Key</a> </b> 0C0A 7486 B97F
92EE AE50 A98C A4F3 087E 8CE9 A782 |
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madscientist
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Samosa: metaphosphoric acid is (HPO<sub>3</sub><sub>n</sub>.
I weep at the sight of flaming acetic anhydride.
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DDTea
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Madscientist- do you mean that Metaphosphoric Acid is a polymer (hence the n) ? If so, would it not be possible to depolymerize it and therefore use
it in reactions? I have read that it is used in the pesticide industry, so I'm quite confident it could somehow be used for our purposes.
If you choose, Phosphoric Acid could be subsituted for Phosphorous Pentoxide. However, by doing this, a lot of HCl is created and has to be removed
from the final product. Also, since vulture and I were discussing means of procuring Phosphorous Pentoxide (by burning of Matchbook strikers in
controlled conditions), we figured we could simply use that. Similarly, if you don't feel like having one "super" poison on hand, you
could work with the two moderate poisons- Carbon Monoxide and Chlorine Gas. However, I figured that with little additional effort (3 more reaction
vessels-1 for the actual reaction, 1 for drying, and 1 for neutralizing the Sulfuric Acid used in the drying process), the Chlorine and Carbon
Monoxide could be combined to Phosgene and make the reaction a lot "cleaner."
EDIT: and yes, I do consider myself a "knowledge junky," as you put it
. I take an interest in dangerous chemicals because a) not many amateur chemists care to work with them, b) there is nothing much I can really
contribute to amateur explosives, and c) it gives you a rush when you succeed in making one .
[Edited on 10-14-03 by Samosa]
[Edited on 10-14-03 by Samosa]
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Iv4
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No interest in actually making it(we right now)but just wanted to check my half ass theory.
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DDTea
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Now that I think about it some more, a much easier way of generating Phosgene is by heating Carbon Tetrachloride and Concentrated Sulfuric Acid
together. Only problem is, I have no clue how to get CCl4 or how expensive it may be.
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vulture
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CCl4 is going to be very hard to get. Even professional chemists need a good reason to be working with it, since it has been labeled as one of the
evil chlorinated carcinogens of death. I leave it to you if it is correct to treat/label it as such...
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Polverone
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J. Chem. Rev.
THE HALOFORM REACTION
REYNOLD C. FUSON AND BEETON A. BULL Department of Chemistry, University of Illinois, Urbana, Illinois
Received September 28, 1934
| Quote: | The haloforms, when prepared by the haloform reaction, are contaminated to a greater or less degree by the corresponding tetrahalomethanes. This is
due to the action of the hypohalites on the haloforms by which the latter are converted into the corresponding tetrahalogen compounds: CHX3 + NaOX =
CX4 + NaOH. This is a general reaction (83, 73, 8, 38); it often becomes the principal reaction when dilute solutions are used. Thus, Wallach (198)
found that in the formation of bromoform from hypobromite and acetone in very dilute solutions, the reaction was slow and that carbon tetrabromide was
the chief product. This influence of the pH on the course of reactions involving hypohalites is frequently noticed (105, 119, 79).
(198) WALLACH: Ann. 276, 149 (1893).
(105) KOLTHOFF: Pharm. Weekbald 62, 652 (1925).
(119) VAN DER LEE: Chem. Weekblad 23, 444 (1926).
(79) HATCHER AND MEELLER: Trans. Roy. SOC. Can. [3] 23, Sect. 3, 35 (1929). |
Perhaps it can be done stepwise too? Preparing CHCl3 from acetone and hypochlorite, then further chlorinating the CHCl3?
I also found a possibly interesting alternative chlorine/chlorination tool: according to the Journal of Applied Chemistry of the USSR (can't
remember specific issue ), calcium hypochlorite + a cobalt salt yields copious
oxygen when heated in aqueous solution. When heated dry, the cobalt + hypochlorite mixture instead yields chlorine. The catalytic effect is even
stronger if a 3:2 mass ratio of cobalt and iron salts is used. I believe they used something like 1 gram of catalyst for 50 grams of calcium
hypochlorite. I think this bears further investigation.
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DDTea
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On another note, sciencelab.com sells Phosphorus Oxychloride in lab size amounts for a rather high price ($180 for 500 ml-- still, for our work, I
don't think we're looking to fill artillery shells or missiles). POCl3 lends itself well to making all sorts of dangerously reactive
Organophosphates... But, after reading a few sections from that Phosphorus/Fluorine Toxic Action book, Phosphorus Oxydichloride Fluoride (whatever
it's called) lends itself even better... The trick is to fluorinate POCl3.
Does anyone know how the Cyanide ion compares to the Fluoride ion in terms of reactivity of Organophosphates?? I hear all sorts of things comparing
Sarin to Tabun- "Tabun is more irritating than Sarin," "Both Tabun and Sarin have poor detection qualities," (i.e.: both are
odorless, both are have no irritating properties) "Tabun is more toxic than Sarin," "Sarin is more toxic than Tabun." I wish
people would get their facts and nomenclature straight- it would make research so much easier
[Edited on 11-10-03 by Samosa]
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madscientist
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Remember that purchases of POCl<sub>3</sub> could be considered highly suspicious due to its use in LSD synthesis.
[Edited on 10-11-2003 by madscientist]
I weep at the sight of flaming acetic anhydride.
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Iv4
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Here's emedecines bit about nerve agents.I think I have some actual tables here somewhere.I'll post them when I find them.
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Al Koholic
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One can produce phosgene very easily from chloroform, sulfuric acid, and heat. No need to bother making CCl4 when CHCl3 is so easily obtained.
Also, something that you might want to consider for phosgene is a gas stream of CO and Cl2. This reacts and I believe can be used directly after
mixing because the reaction is quick. Just lead the gases together into a tube which leads to your main purpose, ie: bubbling it through something...
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vulture
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Phosgene will decompose above 300C, so that would suggest the formation is exothermic. So leading it through a second reactor with a cold trap might
grealty improve yield.
And of course higher pressure, 2molecules of gas --> 1 molecule, le chatelier.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Al Koholic
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Indeed indeed! Also, the boiling point of phosgene is a modest 8C so there should be no trouble at all cooling it to the point of condensation.
Hell, if you do the prep in a garage in the dead of winter, ie: -25C, you should be able to collect the liquid with no problem from a distillation.
This is probably much easier to deal with than the gas in some apps, more difficult in others....the point is you have an easy choice.
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fritz
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I want to add that the for reacting CO with Cl2 the apparatus shuold be exposed to sunlight(UV-light) or you let the mixed gases stream in a tube
over activated carbon(cooling(!) the tube to 250°C) Phosgene could be made free of Cl2 by streaming over Sb.
Other methods are:
-Soda+PCl5
-heating Chloro-formic acid trichloro-methylester at 340-340 degree C
-CO+SbCl5(hot)
for storage the use of Chloro-formic acid trichloro-methylester might be preferable, since it´s a liquid (b.p. 127,5°C) this stuff is also called
diphosgene. I have unfortunatelly only spare information about synthesizing:
-reacting HCOOH and MeOH
-photocatalysated chlorination
but I could tell you where to find this substance in the Beilstein-enceclopedia:
EIV3, 33 I hope this could help!
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DDTea
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Chloroformic Acid, Trichloromethyl Ester is more popularly known as Trichloromethyl Chloroformate . It is prepared by bubbling Chlorine through Methyl Formate; however, there are impurities by this route (mono- and
dichloromethyl Chloroformate). The temperature is at first maintained at 30*C by a slow current of Chlorine, and then the stream increased and the
temperature is gradually increased to 90*C. Also, UV light is very important in this reaction. To separate the impurities, the product should be
distilled. The yield is 70% of the theoretical. This is according to The War Gases.
To me, this sounds like a candidate for Electrolysis. I imagine we'd want an excess of Chlorine gas too, so as to completely chlorinate the
Methyl Formate.
I also remember a crude method to generate Phosgene on E&W-- by adding Methylene Chloride (CH2Cl2) to Gasoline and then burning it. However,
since CCl4 and CHCl3 like to form Phosgene on reaction with Sulfuric Acid, could the same apply to Methylene Chloride, which is readily sold OTC?
[Edited on 12-13-03 by Samosa]
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guaguanco
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| Quote: | Originally posted by vulture
CCl4 is going to be very hard to get. Even professional chemists need a good reason to be working with it, since it has been labeled as one of the
evil chlorinated carcinogens of death. I leave it to you if it is correct to treat/label it as such... |
Well, it's by far one of the more toxic halocarbons; it reaks havoc on the liver. It's not as bad as sarin, but it's bad news.
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