Al/Hg/Nitro in a bucket

[baalchemist]

Baal was feeling a little adventurous and tried running one of these reactions in a 5 gal plastic bucket and it worked rather well I must say. First off a 5 gal. plastic bucket was nested into another bucket of the same dimensions,and 1.5L-MeOH & 1L-99%IPA was added along with a 3" stirbar. Keep in mind that the ambient air temp is ~0c, anyhow 15g of Al was added w/100mg-HgCl2 and stirred on high. 100g-Ketone & 80ml-nitro & 100ml-MeOH were mixed together and slowly dripped into bucket. A fan was placed blowing on the side of the bucket the whole time. As the foil broke down, new foil was added in 5g allotments(120g's total), and the addition rate of reactants was paced accordingly to keep the reaction intensity(mild) somewhat controlled. After 45 mins addition was completed and the was fan shut off, then this was left to stir for ~4hrs. Added 2L-Toluene & slowly added 2L-35%NaOH, stirred for 30 mins. Allowed layers to seperate and top layer was removed and washed with brine & H2O, then dried w/MgSO4.  After gassing, a yield of 85g's MDMA>MP-149C.
Small additions of MeOH were added during the addition process to help replenish, and the lid was loosely fitted to the top of the bucket also. All in all it was'nt that stinky of a reaction, of course until you base the post reaction mix. The two buckets are a must, the reaction bucket gets a little flexible from the heat in the initial part of the reaction. Definately a very unconventional method, but it'll work in a pinch. I'd like to run one in an Al bucket nested in a plastic one. Run it with a continuous drip until the Al bucket is shot.   
GODISNOWHERE

[Antibody2]

buckets make all kinds of sense

[baalchemist]

Definately a 'winter' reaction, in the summer forget it.
GODISNOWHERE

[terbium]

buckets make all kinds of sense

Courtesy of PolytheneSam  Post 243138 (not existing)

[baalchemist]

Shulgin seems to compare it to Mescaline in its effects. Thats sounds cool to me, I wonder if it'll make you grow a hump or not? I get nervous in unexplored ground, but hell its easy enough to make. I wonder what other oils can be run through the same exact protocol?
Edit LT/: He meant this to post here:

Post 250853

(baalchemist: "Re: Bioassays", Methods Discourse), but it landed mistakenly first here, for those who don't understand where he is talking suddenly about   .
GODISNOWHERE

[sunlight]

Good finding, happy cooking. I like specially you used 100 mm Hg for 120 gr of Al. In other hand take care with methanol vapours. The damage is acumulative.

[LaBTop]

"Dripping in" of alu foil, see

Post 224697

(LaBTop: "Re: Making Clear", Methods Discourse), so it works as expected. Now try alu powder added with a powder funnel.
Should bring your alu consumption back to very acceptable minimal quantities.
You see, it's advantageous to be drunk on a regular basis.   LT/

Btw, if those 1 on 15 and 1 on 10 ratios of ketone to solvents could be brought back to normal quantities, then you have your "Most wanted" Hive procedure! Good work!

Btw2: In summer, put your bucket and the whole stirrer setup in an open freezer, the cold air will stay inside if you use only a PC exhaust fan to blow cold air to the bottom of the bucket. Cold air is much denser than warm air.
If you can buy a small camping freezer, fill the bottom with car-antifreeze up till 10-20 cm, use an overhead stirrer, and put your bucket in there, the freezer will work much better that way, only choose your quantity of antifreeze carefully, if too much, the freezer will have to work too hard, overheats it's compressor and shuts down or simply burns out when it has no overheating breaker device.
Bin there, done that, works FINE! Slowly increment the freezers knob settings to give the compressor time to adjust to the antifreeze temp. They are meant to cool AIR, you know, but you can fool them this way. Clever ones precool their antifreeze!
Look for a freezer which doesn't have it's coils fit all the way up along the walls, then the coils which are above the antifreeze level will get HOT! Older types cool only the bottom. LT/
WISDOMwillWIN

[LaBTop]

If this is thought out cleverly, it can be done at MUCH bigger scale.   LT/
WISDOMwillWIN

[Osmium]

I fail to see the advantage over using a condensor to keep the MeNH2 inside.

[baalchemist]

My previous post went into the wrong thread, what was I thinking?
There is really no advantage Osmium, the lower yields reflect that. Apparently there probably wasnt that much MeNH2 lost. I theorize that this type of reaction utilizes the reactants immediately(as available) and gives the MeNH2 little or no time to escape, unless of course it becomes a
turbulent runaway reaction.
GODISNOWHERE

[RollWitMe]

I see one, I never had anything over a 2L 3 neck RB flask.
It's much easier to scale up using this procedure and lots of caution. 55 Gallon Trash Cans come to mind. Imagine splashing around in a kiddie pool filled with ice and water while you splash the cold water onto the can while a huge fan blows the MeOH vapors into your neighbors kitchen. I suggest also using a pool pump and running a cooling coil INSIDE the can. Teflon tubing would be safe. run about 50 feet of it for some extreme cooling power from a kiddie pool filled with ice.
I like to cook! . . . but some dudes in blue vests with yellow letters took my kitchen.

[Osmium]

> There is really no advantage Osmium, the lower yields reflect that.

I meant LT's freezer idea.

> It's much easier to scale up using this procedure and
> lots of caution. 55 Gallon Trash Cans come to mind.
> Imagine splashing around in a kiddie pool filled with ice
> and water while you splash the cold water onto the can
> while a huge fan blows the MeOH vapors into your
> neighbors kitchen.

Oh my god. When trying to do X00g or even multi-kilo batches I suggest you look into sheet Al or hydrogenation, not Al foil. Even when using foil a stirrer will be needed, and I don't see any reason why a condenser should be omitted.
What if your yield is 100g lower than it could be since you left out the reflux condenser? Is that worth it to you? You do the math...

[RollWitMe]

Hmm, 100g = ~3.75 ounces = $7,500 bulk sale. Of course if you lose 100g out of a 2Kg batch in a bulk sale that 100g is only worth $4,500 - $5,000 . out of $125,000.  Eh, whatever, most of you people are research chemists screaming & crying about yield. I've done and currently do production chemistry dealing with 400-500Kg of organic oils. I really don't care if I leave out 4 Litres of tail cuts after I've already distilled 350KG of product. I know this doesn't relate to using a condensor, but if you do what I said and run tubing through your bucket with a pool pump and ice water, a pool pump moves ALOT of water. should keep it cool. Also, stirring would be overhead stirring which i just assumed people would do
I like to cook! . . . but some dudes in blue vests with yellow letters took my kitchen.

[Goodtimes]

Yes!!

Finally, a backup plan incase the 3-n flask breaks...

very inventive baal!!

great!  
"The gods are too fond of a joke."  (Aristotle)

[LaBTop]

Oh my god. When trying to do X00g or even multi-kilo batches I suggest you look into sheet Al or hydrogenation, not Al foil. Even when using foil a stirrer will be needed, and I don't see any reason why a condenser should be omitted.

You still go out from the basic idea, having all your alu already in the motherliquids.
My idea of using Alu powder is based on the context of this thread: "dripping in" alu.
And if that works, you have the most OTC procedure ever seen here! From small to bigscale, and bigscale I mean kilo's of ketone.

I suppose you could bring back all those immens quantities of solvents (MeOH,IPA) to very acceptable bigscale quantities when regulating the "dripping" rate of the Alu powder.
The amount of nitro and HgCl2 is already very acceptable, so could someone tell me why alu powder shouldn't work?
Combined ofcourse with a nearly closed system with an overhead stirrer and a reflux column added.
That freezer idea was just to show the "all weather" possibilities for rough fieldwork.

I'm glad Baal took the time to try out such a "crazy"idea! I hope he will try the powder also.
I'm quite sure it will work when the pace of the alupowderdripping is controlled carefully by a thermometer coupled to a  powderfunnel opening device. Tests can be done by hand with a pipette.
The surface to mass ratio of alupowder is immensly bigger than sheets or foils. LT/

WISDOMwillWIN

[baalchemist]

Baal has a storage shed packed to the hilt with lab glassware for all occasions, but there are times when the allure of that $2.99 plastic bucket cannot be overcome,haha.
Cumulative effects you say... well Baal had no intentions of reproducing anyhow.
GODISNOWHERE

[unnilhexium]

Outstanding post Baal!  The "dripping in of aluminum" has given SWIM an idea.  Recently, SWIM, having no MeAm source, but plenty of NH3HCl on hand, took that route to MDA.  Whenever the Al/Hg was spent, the reaction still reeked of NH3, and the pre-A/B xylene extraction was extremely yellow, indicating a lot of unreacted MDP2P.  Yields sucked, as expected, but 9 out of 10 villagers prefered the MDA, so now SWIM wants to make MDA instead.  The idea is, to use less foil initially, and to "drip in" the foil over the course of several days, and using a very small amount of mercury salt.  Any thoughts?  SWIM is going to try this whenever he finds time, and see if yields improve appreciably.
106

[Antibody2]

there is no need to operate at refulx, my favorite rxn vessel is a 4l beaker, and if it gets frothy set a 2l flask full of cold water on top, or a fruit bowl etc, but some rxn are better kept at RT, depends what you are doing

[baalchemist]

Running an Al/Hg over a period of days with periodic Al. additions to increase MDA yields> How do you figure that might happen? I would guess it as a waste of time & chems, definately would look for a more logical route.
GODISNOWHERE

[unnilhexium]

The logic behind that was, that the yields from that reaction are poor because the aluminum is used up too quickly, and is expended before it can aminate more than about 20% of the mdp2p present, due to nh3 not being as reactive as methylamine or ethylamine.  I figured that adding more aluminum as it is spent, would continue to react all of the unused mdp2p and nh3, thereby increasing yields.  Albeit, it may require a lot of aluminum and solvent by the end, but until swim can find a better way, swim would be happy if ~60% yields could be attained.  Swim is going to try a micro-batch in the near future, just to see what happens.
106

[psychokitty]

According to an old Al/Hg thread from waaaaay back when, one bee indicated that the powder addition method does indeed work.  But there were no experimental conditions indicated.

IMHO, adding Al foil in increments should work just as well.  This way, the exothermic nature of the reaction is better controlled and stirring can be easily accomplished.  Al foil is OTC.  Al powder is not.

[foxy2]

Someone needs to try LT's idea!!!!


Or how about this.
Run the reaction flowing thru a pipe.

(Fuck, I just read the other post on Al/Hg's and it seems my idea won't work due oxide formation)
My original idea was using AL tubing or a thin SS pipe packed good and tight with Aluminum wire.  An old HPLC pump would run the system perfectly.  The pumps are not cheap but you can find some good deals.  You could try running at higher temps and pressures.  You would have tons of control over all the variables except the state of that damn Al. If this worked you could do multi kilos run easily. 


It might bee possible to feed all the reactants,(Al powder slurry) to the pipe for reaction.    Feeding the slurry would definately bee a bitch. And I almost forgot about the AL sludge, it would probably clog everything up.  

Foxy STILL needs to get laid!!!

[brownhornet]

well happy new year to all.  LT talks of large scale al/hg nitro; using al sheeting/powder added to entire reaction mix. my questions and comments;
when u say entire reaction contents assumming everything except al; ie nitro, tone, hg, meoh, right?
-well then u can see how how exothermic variable that can run off can be controlled.
-appears highest yeilds were obtained when reaction was run at a very violent rate. scary no need to breath hg contaminated vapours.
-well could eliminate chance of runoff if reaction is heated and held at reflux and al added to this. not only would this eliminate runoff (provided u add al at a consumable rate) but it would meet the requirement of vigorous heat conditions for highest yeilds.
u could of course also control reaction if al rods or sheeting is submerged in reaction contents. turnoff stirring and one would expected to see fizzing at surface of submerged.  if reflux begins to run at a higher rate than needed then pull out submerged al rod/sheeting.
-would the hgcl be consumed or become inactive in this process requiring further addition? im guessin not
-how much mass of al sheeting/rod need to be consumed to completed reaction. i know its more a matter of surface area but is there any indication that ketone has been aminated entirely.
-would running a reaction in kg quantities hurt the yeilds if it is run past its completion. seems mm's al/hg gave better yeilds when running past when fizzing has slowed and started cooling. ie will reflux heat destroy product after its formed.
-would it bee a good idea to strip surface of sheeting/rod with 5%naoh before submerging/amalgamating.
another advantage here would bee the exposed al sheeting/rods would not have their surfaces covered from sludge of consumed al since they are suspended.
of course this would bee done with a ss cold h2o coil above it, all running under a fume hood.

ps together we can rid the world of its misery with more honey

[Osmium]

Yeah, let's reinvent the wheel.

[foxy2]

Good Idea Osmium

I was just having fun thinking out loud. 


Foxy is doin just fine.

[Antibody2]

why do some people look at wheels as though they are a fait accomplis?. the tire companies certainly haven't, don't hear anyone laughing at them.