Sorry Antoncho - No H3PO4

[methymouse]

In

Post 301629

(Antoncho: "Two tried-and-true ways to make MeI !", Chemistry Discourse) Antoncho describes two methods for making MeI, and the excellent rating it received was surely well deserved.  Regarding Vitus' method for the generation of MeI from aluminum triiodide, methanol and sulfuric acid, he writes:

"Sidenote: should bee much better with usage of H3PO4, don't you think so? It would react w/AlI3 quantitatively w/out any oxidation!"

This is a nice thought, and I thought so as well.  Unfortunately, when SWIM tried it, he got methanol in the receiving flask and nothing else.  I believe that the temperatures required to make HI in this fashion are higher than the boiling point of methanol, and so you would have to make the HI first, then add the methanol.   

All is not lost in SWIM's experiment, though.  He added some H2SO4, and is currently distilling MeI, which will of course be used for fumigation, not anything illegal.   

[Vitus_Verdegast]

Regarding Vitus' method for the generation of MeI

You mean Vitsh of course.
As far as I know, I have not written a method for generation of MeI   .

BTW, methyl iodide for fumigation you say.. Isn't that outlawed in most countries?  

[methymouse]

Yes, of course I meant Vitsch, sorry about that.

My understanding of the legal situation surrounding MeI is that it is currently in the regulatory pipeline in the US.  I believe that they first banned MeCl, which was promptly replaced with MeBr, which took several years to ban.  That was then promptly replaced by MeI.  Fortunately, this can't continue unless orchard owners happen to have particle accelerators...

BTW, SWIM's yields were extremely poor, probably from the low concentration of HI.  Some of the AlI3 was oxidized to elemental iodine by the sulfuric acid, yielding a so-purple-it's black distilling flask.  Sigh.  At least the I2 can be recovered with SWIM's next batch of tincture.

Added later:  SWIM had some difficulty extracting the MeI with a syringe due to the extreme volatility of the compound.  Like ether and the like, it squirts out if you're not careful.  I strongly suggest prechilling your syringe in the freezer for a while before extracting.

[hest]

Fortunately, this can't continue unless orchard owners happen to have particle accelerators...

That was a good one