Methylphosphonyl difluoride

I'm very interested in nerve agents and their synthesis, but I don't plan to make any soon.... I don't have nearly enough equipment. I don't even have a proper set of gloves yet

I was just thinking, would this pathway for synthesis of the Sarin (GB) Precursor, Methylphosphonyl difluoride be acceptable? If you wanted to make Methylphosphonyl dichloride instead, would it still be possible with this pathway?

I was thinking of this:

Take some monopotassium phosphite (fertilizer) and add H2SO4 or HCl to it to yield phosphonic acid and a salt

Distill out the phosphonic acid (BP at 164 F) from the KCl, and dry the product just in case water ends up on the phosphonic acid

Mix equimolar proportions of methanol and a solution of phosphonic acid with a dilute H2SO4 catalyst and reflux or stir as needed

Add the methyl ester of phosphonic acid with double the molar amount of Hydrofluoric acid (a concentrated solution) and stir

Dry out water -- Then the methylphosphonyl difluoride should be left...


How flawed does this sound? I'm just curious.

Personally I would never attempt the synthesis of ANY nerve agents, Lewisites, etc. Not only because of there extreme toxicity, but also because doing so without a proper licence would be extremely illegal. Well then again that would be considered MADscience.

Now I see a couple problems with you procedure. First of all I fairly certain that esterification is not going to work, and the reason is many organophosphates tend to undergo hydrolysis in the presence of water. So as soon as any of your methyl ester forms it will probably be hydrolyzed by the water generated in the reaction. But I may be wrong here so feel free to correct me if I am.

The final problem I see is the HF, your going to need some very specialized equipment for that (PTFE) and I doubt thats going to be easy to get or cheap. Also HF is really toxic, de- calcifying bones...
But if none that turns out to be a problem then you look good to go!
Good luck, don't poison yourself and the entire city you live in

Quote: Originally posted by Rich_Insane

I'm very interested in nerve agents and their synthesis, but I don't plan to make any soon.

Well I'm not planning to make this. First of all, I'm a minor, no way in hell I could acquire all the safety equipment to make this. As for the legal aspect.... doesn't matter much to me, not to sound like an idiot. I would never synthesize over 10 mls.... and I'd probably destroy the product before a week. And I did do a search, but the search engine really bothers me.

Well, I looked up the methyl ester and it does exist.... What if l one were to reflux the mixture of phosphonic acid and methanol with a drying apparatus?

I'm also very confused now, because Wikipedia says that you just need equivalent amounts of methanol to form the methyl ester. Does that mean that you want this:



Instead of this:



The first one actually works better because then the hydrogen could be ripped off to make the hydroxyl on methanol into water..... And those two hydroxyl groups could be removed with HF to form water. I'm just wondering, because logically, you would form dimethyl phosphonate,just since you have less methanol, you would only produce half the yield because there's not enough methyl groups to go around.

But is it possible to synthesize these pesticides with just gloves, some basic glassware (no condenser yet..... no parts for my reflux condenser), and the outdoors as ventilation? I have this strange attraction to organophosphates, I'm not sure why

Quote: Originally posted by Rich_Insane

I have this strange attraction to organophosphates, I'm not sure why

I can't get very much equipment as I'm a pretty cheap/poor person, but I have a certain detraction for inorganic chemistry other than the beautiful colors, so I only really like organic chemistry, and since everyone has a thirst for synthesizing something significant or dangerous (Don't deny it ), I guess organophosphates really appeal. I like acetylcholinestrase inhibitors a lot too. Of course, most organophosphates do something or another to harm cholinestrase or acetylcholinestrase levels.

Two problems with me are: Cost, and Availability. There seems to be a lack of companies that will sell cheap reagents and glassware, let alone to an individual.

Also, considering that I'm a minor who gets little to no income, I'm fairly poor. That's why I mostly like esterification reactions. Concerning nerve agents: Sarin is surprisingly simple to make..... That's how Aum Shinrikyo was able to make so much of it with the guidance of a single graduate of Organic Chemistry. I can't imagine how they got enough money to purchase 10-inch thick fume hoods for the final steps of the synthesis.

I just said that I didn't ever plan on doing this (read all of my poasts)..... I'm curious at the synth of organophosphates.... In a way this is mental masturbation, perhaps the good kind

And this is a viable synth in my opinion..... Before anyone gets ignorant and forgets to read 75% of my posts on this thread: I do NOT plan to make this...

It is a published procedure for making small amounts of isotopically labelled Sarin.
There are probably other reagents you could use in some of the steps.
The critical step is step 2 that introduces the carbon phosphorous bond.
Bearing in mind the toxicity of DF and the fact that being caught with even tiny quantities of it outside a licenced facility could result in a one way ticket to some hell hole it is not practical mad science in my opinion.
If you poisoned yourself and presented at the local A&E and they picked it up with GC - Mass Spec, the men with dark suits and wrap round black glasses would be sitting at the end of your bed while you were recovering.
After that it could be pliars on your toenails or a lecky battery on your man berries / lady bits

That is a modification of the Michaelis - Arbusov reaction.
Small amounts of the alkyl phosphite are converted to the alkyl iodide that then attacks the remainder of the substrate to form the alkyl phosphonate ester.
The ester can be directly cleaved to the dichloro methyl phosphonate without the hydrolysis step.
It should be pointed out that attempting this may result in injury, death or an indefinite stay in the highest security slammer that your country has.