MM Nitro/Al-Hg variation: No HgCl2

[isohuman]

ISO-SWIM decided to try a new twist on the Methyl Man Nitro writeup.  ISO-SWIM decided that instead of using HgCl2, he would try Hg(2?)I2 instead(mercury blobs dropped into I2 tincture, ala unnilhexium).  The batch was done at a half scale, 12.5g ketone, 10ml MeNO2 and 13.7g aluminum foil.  The tincture, .24g Hg from a thermometer dropped in a 30ml 3% I2 tincture 1 week earlier, was dissolved in 400ml MeOH, and dumped into a 2L RB flask, to which the aluminum and a 2.5 inch stirbar had already been added.  Amalgamation took approximately 35-40 minutes, and once complete, the ketone/nitro was dripped in.  Do not wash the aluminum after amalgamation, this was tried and resulted in a failed run, without ever heating up appreciably during the addition.  The ketone was dripped in over the course of about 15 minutes, and the reaction proceeded as expected, and reached an impressive reflux.  The rest of the procedure was carried out as MMs writeup, and yielded 10.9g of the hcl salt.  Just in time for the weekend

[PoohBear4Ever]

Thank you for trying this:      

Props go out to unnilhexium,

PB

[TranceMe]

The tincture, .24g Hg from a thermometer dropped in a 30ml 3% I2 tincture

Oh my, oh my!! And that's it? Life keeps getting easier and easier

Chemically enhanced.

[goiterjoe]

um, won't mercury in the elemental form amalgate aluminum?  People just tend to use the chlorine salt form because it makes the reaction run faster and clean up easier.
If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music

[Rhodium]

joe: The amalgamation would not be even and dead slow. Compare the area of 0.1g dissolved HgCl2 to the area of 0.1g solid Hg. Big difference, right?

[TranceMe]

(mercury blobs dropped into I2 tincture, ala unnilhexium)

Can you please point me to this post? I can't find it UTFSE.

Chemically enhanced.

[bicepules]

     Yes, yes I to would like to see a little more here to.  Came up with nothing UTFSE. 
"No I'll tell you what insanity is, insanity is majority rules"

[noj]

I believe it came from TSII. Do a search on "HgI2" if you need information. BrightStar mentioned it being the least desireable of the Hg salts for amalgamation, but that was in relation to water solubility. Hellman had a thread on it several years ago, but it has been purged.
Real men cook naked.

[isohuman]

I guess TFSE isn't working properly, I couldn't find the post, but it was on a thread about peracetic acid, where unnilhexium made mention of his amination technique using I2 tincture.  I don't know if that was a unnilhexium original or not, he was just the first bee I saw posting about it.  Anyhow, for those of you worried about side reactions, the residual I2 seems to form some kind of alu-halide, as the red color leaves the solution during the amalgamation.  Also, the tincture adds about 15ml of water to the reaction, which should keep Osmium off your case   BTW, it important to periodically shake the tincture bottle, to break up the mercury blob so that it can react.  Also, make them as far in advance as possible.  They can be made weeks, months or years in advance, IT'S JUST TOO EASY!!!!!!!!!!!!!  Isn't that so much nicer than making or buying HgCl2?

[mushhead]

Wow!  If this works as advertised, SWIM will be a very happy person.

By UTFSE, I found a couple of posts from hellman.  He didn't give much detail but insists it works. 

Here's a couple of posts

Post 104506 (missing)

(lost in the sauce: "Re: HgI2", Chemistry Discourse)

Post 106043 (missing)

(hellman: "Re: HgI2", Chemistry Discourse)

[noj]

Seems like a waste of I2 if you ask me. HgCl2 is pretty cheap to buy. But if you have the elemental Hg I guess this would be nice.
Real men cook naked.

[Vibrating_Lights]

use 1 rectal thermometer per 1 oz bopttle of 2%iodine.  exess won't hurt.
VL_

[isohuman]

I found it

Post 248601

(unnilhexium: "Re: When substituting GAA for Formic acid...", Chemistry Discourse)

However, it doesn't give too much detail either.
LT/: it's [xxxxxxx] which translates to

Post 248601

(unnilhexium: "Re: When substituting GAA for Formic acid...", Chemistry Discourse)

[PoohBear4Ever]

Heh, LT, that took me a second to process...

Time for some sleep,

PB

[SuperStar]

I have a few questions. 
One rectal thermometer into 30ml 2% then use 2 of these bottles for 25g Al?  What is the exact ratio of tincture to Al?

If the tincture does not convert all the Hg to salt (excess Hg) what are the dangers of the vapors during reflux?

I am a little slow so details help.

[noj]

wow, that would be way too much mercury. You only need 100mg of Hg salt, at most 200mg, for 27g foil.
there must be an answer for everything, if only you knew how to set forth the questions

[SuperStar]

Like I said, I'm a little slow   .

So how much tincture? (ml?)  I assume approx 250mg Hg per bottle. So is the Hg converted equally to salt?  250mg Hg in equals 250mg HgI2 per bottle, would this be correct?

I guess my big question is how to convert the ml of tincture (using 1 thermom per 30ml) to grams of Hg Salt?

[PoohBear4Ever]

So is the Hg converted equally to salt?  250mg Hg in equals 250mg HgI2 per bottle, would this be correct?

No, but from what I've read, using about 0.5g blob of Hg in one bottle is good for ~ 30g Al...

PB

edit:  Hg= 200.59/mol = A;  I= 126.90/mol = B;  HgI2 = A+2B...

[cheeseboy]

Come on SuperStar, live up to your name.
May The Source Bee With You....Always.

  - OB1KNoBee

[SuperStar]

Work with me, I am trying to get with the program.  Just so you know that was my first post.

So let me sum up.  We are assuming approx .5g Hg per thermometer added to 30ml 2% tincture. Add 30ml of this tincture for ~ 30g Al.  Sounds easy enough.  Oh yea, Shake tincture well and let stand for about a week.