bucket reductive animation

[GOD]

regarding the bucket animation on Rhodiums site:

A 'dropping funnel' will suffice in place of an addition funnel for this set-up correct? after all, there is an opening from the other unconnected end of the cleisen adapter to regulate pressure- or is there something swim is missing here?
also, does a vigreux column nessisarily have to bee used? what about using a different column, just so long as they add up to 400" ? 
My mom tells me Im good lookin'!!!

[PolytheneSam]

Suspended animation or ketone amination?

http://www.angelfire.com/fl/twilightzonelist

http://www.geocities.com/dritte123/PSPF.html
The hardest thing to explain is the obvious

[GOD]

oops on the spelling.

thanks hooked.

when someone asks what the sound of one hand clapping sounds like, you should smack them in the ear.

[Vibrating_Lights]

Sswim does his additions with a pyrex measuring cup. It really doesn't matter. If it gets too hot then put some ice on the lid then you got oa whole shitload of cooling surface.
Vl_

[greeter]

1)  I don't see this in the photos but presumably you set the bucket on your magnetic stirrer, right?
2)  What size stir bar works best in the bucket?
3)  The 'shank washer' fits 24/40 glassware or something else?
4)  Any reason why you shouldn't put the addition funnel into another hole in the bucket lid (as opposed to the top of the column)?

thx

Oh yeah, and:

What do you do with all the sludge when the reaction is done?  (seriously)

A watched pot will indeed boil.

[cheeseboy]

Bucket=Oxone run??? Just wonfdering wtf this is all about.Peeeeece
Bubba Fatt - LA's Biggest Bounty Hunter. His subjects are at large and so is HE!

edit, oh aminate.sorry, cyabo?

[lugh]

What do you do with all the sludge when the reaction is done?

Post 228769

(lugh: "Re: proper waste disposal", Chemistry Discourse)

Post 228816

(foxy2: "Re: propper waste disposal", Chemistry Discourse) &

Post 229212

(foxy2: "Re: propper waste disposal", Chemistry Discourse)  

 

[PrimoPyro]

Bucket=Oxone run??? Just wonfdering wtf this is all about.Peeeeece

It's the Methyl Man Aluminum Amalgam Reductive Amination with Nitromethane, done in a bucket instead of traditional glassware. The reaction is often cited as the MM Al/Hg w/MeNO2 for shorthand.

                                                   PrimoPyro

[Vibrating_Lights]

Dump the sludge in your local pertroleum recycling bin.
3" stirr bar is great 2.5 will suffice.

[greeter]

done in a bucket instead of traditional glassware

Cheese, you've probably read (done ;-) the MM amination.  The recipe calls for a 2L flask.  The bucket is a 7.5L vessel and it's very cheap to build, so you can scale the reaction up easily.  The pics of it are in the Chemistry section of Rhodium's site, look in the Multimedia area.

Now one more question for those of those who have run this...

The 'recent' commentary regarding the MM Al/Hg (esp. baalchemist's process) suggest continuing the reaction with external heat for 3.5 hours post addition.  I take it none of you are doing this step?  Is it even necessary?  What kind of yields are you getting?

-g
A watched pot will indeed boil.

[noj]

If you allow the sludge to sit, until the solution turns clear yellow, you will see a bead of mercury at the bottom. RECOVER!
Mastery is based on the understanding and practice of technique.

[cheeseboy]

greeter..
never tried a methyl man amination, never even seen nitro. Cheese has only ever reduced store bought ketone a few times to MDMA/MDA via methylamine/cyano- ammonium acetate/cyano. Oxone ketone has been made yet amination failed. Back to the 'ol drawing board if i can ever get it together and get more safrole. Going to ditch the Oxone method and go Formic.Sounds better, more tried and true. Plus yields will be better i hear. Cheers.
Bubba Fatt - LA's Biggest Bounty Hunter. His subjects are at large and so is HE!

[Vibrating_Lights]

There is no need for additional heating.  Buckets are the shit and come in all sizes up to xxxliters.  glass will shatter, plastic will not.  A coldfinger can be built into the top of the bucket to improve cooling.ohhh A better work up than M/M is osiums workup of the Al/Hg in adding just enough NaOH to free the MeAm.  Basify till the MeAm starts bubbling then stir for 2 hrs.  when stirring stops all the Al sludge will fall to the bottom quickly. Pour off the liquid and extract sludge with Alcohol a few times.then add enough water to make the liquid white and extract with NP.
VL_

[dr_ruthenium]

VL: Are you referring to Os's Al/Hg on Rh's page?  You say add enough NaOH to free MeNH3.  Do you mean from MeNH3-HCl?  'Cause that's not work up.  Maybe you could referrence Os's post for that w/u.  I know that MM's w/u needs an A/B, but other than that I thought it was good.
TRISMUS!!!

[greeter]

If you allow the sludge to sit, until the solution turns clear yellow, you will see a bead of mercury at the bottom. RECOVER!

Have you tried adding aluminum strips to the sludge and allowing them to sit for 8 hours or so?  The posts that lugh reference above indicate that all the Hg will ultimately amalgamate back to elemental Hg in the presense of aluminum strips.  Now maybe the amount of aluminum used in the reaction is enough to convert ALL the HgCl2, I don't know.  Anyway, it might help to recover more mercury (disclaimer: this is blatant speculation on my part).

Ok, second question...

The bucket amination calls for 800mg HgCl2.  I realize that everything from the MM synth was scaled 2x, but is it really necessary to scale the HgCl2?  It seems from what I've read that you'd do just as well to leave it at 400mg.

A watched pot will indeed boil.

[PrimoPyro]

1.The Hg cation is much higher in mass than that of Al.

2.There are 2 Cl anions per Hg cation, but 3 Cl anions per Al cation.

3.There are several grams of Al in the system, yet under 1 gram HgCl2

Based on my observations here, I personally believe that the there would be more than enough Al present to completely reduce all 800mg HgCl2 to elemental Hg metal.

                                                   PrimoPyro

[dr_ruthenium]

It doesn't matter if the 2x MM is carried out in a bucket or 6 liter flask, you don't need to double the Hg.  In fact, try using 250mg instead of 400mg.  Then you'll need to add less Al strips!
TRISMUS!!!

[Vibrating_Lights]

Think outside the damn box
 In Mm write up there is alot of NaOh added.  this leaves yo u with a sloution that is prone to emulsions com time for the extraction.  If a smaller ammount of NaOh is used then the al will crash out in a pristine manner which apoun filtration will leave you with a clear solution that will seperate quickly.  filtration is very fast or just pour off the liquid and extract the sludge with more alcohol. If one was to pay attention during basification then they would notice that once a certin point is reached the MeAm starts to bubble out vigerously.  Stop here to filter the al.
VL_

[greeter]

Swim is thinking of running the Al/Hg in a 5gal bucket (~19L) at 4X the MM scale (i.e. 100g ketone).  He would like to know if a 3" stirbar with mag stirring is sufficient or if overhead stirring will be required.  Has anyone tried this?

PS:  Swim is using a 400mm west condenser sitting on top of two vigreux columns totalling 600mm with an industrial strength fan blowing across the columns.  This was massive overkill on the MM at normal scale in a 2L flask, he presumes it will be sufficient to contain the rxn at 4X, especially considering that the 5gal bucket has a lot of room.  Anyone care to comment?

-g 
A watched pot will indeed boil.

[Vibrating_Lights]

A three inch bar will be more than suficent.  You are good to go.
\VL_