Large Scale MM 5-6x ...

[overclock]

SWIM recently dreamed he obtained a 12L RB Reaction flask and a 12L Sep Funnel (Actually a 12L RB Reaction flask with a stopcock and a pouroff valve on the bottem, but works just as well, now he just needs to dream a  heating mantle /w a hole in the middle and overhead stirrer )anyways ...

SWIM was dreaming about a 125ml of excellent imaginary Ketone sitting in this imaginary freezer. In his dream he wanted to convert all the imaginary Ketone to imaginary goodies ah la MM and pack imaginary things up for a bit while he relocates to another imaginary location ...

Questions SWIM remembers from his dream:

1) He has a good magnetic stirrer and several large magnetic stirbars. Would this be sufficent with manual stirring if necessary?

2) He has 2x 300mm Allihn condensers and a 400mm Allihn condenser. Should he hook 2 up inline, considering the volume of the reaction?

3) Is there a risk of explosion on this scale? Stupid question, he knows, but he's paranoid even in dreams.

Thats about all he can remember from his dream. Please let him know about trials and tribulations other SWIY may have encountered in dreams concerning large scale MM nitro ...

Peace.
-OC
"We can't solve problems by using the same kind of thinking we used when we created them."

[noj]

A 3" stirbar worked fine with a 6x Amalgam reduction in a bucket. For that experiement the aluminum was quickly crumpled into 1/2" balls rather than grinding up in a coffee grinder. This allows them to float and puts less strain on the magnet.

Use the 2 condensers inline using ice water.

You control the reaction rate with the addition of the ketone/nitromethane. No risk of explosion if you drip it in about 2 drops a second at that scale, and watch the reaction.
there's a big difference between criticizing your government and criticizing your country

[El_Zorro]

I think it would be a better idea to use something thicker than aluminum foil in a large reaction.  The foil could very easily run the reaction hot, and you could paint you cieling with some Hg solution if you're not careful.  I would suggest cut-up pie pans or flashing.
Who is that masked man?

[overclock]

In SWIMS dream he has a 12L reaction flask, thats 7L of headroom and will be using 700mm of ICE cold condensing (and he can add another 700mm if need be). He thinks an explosion would occur before the reaction would get out of hand. SWIM also knarls his nuggets up tight with a bean grinder which inherently slows the reaction some. MM's writeup is awesome, I think SWIM was just being paranoid again.

Thanks for the advice.

Peace.
-OC

PS. On a side note, for those that are reading this thread, here's a funny little story (well at least as I remember the dream looking back)

SWIM had just got done dreaming about some HgCl2 that would inherently be used in an amalgam. This was the first synth SWIM had ever dreamed about and was very anxious. Everything went w/o a hitch and he decided to "test the quality" so to speak. He prepared about 30g of 1" tinfoil squares, put it in a 2L flask /w 500ml of DH2O, and grabbed his spatula. He opened his bottle of HgCl2 and scooped up some on the spatula and was gonna tap the spatula and dash off a pinch into 2L EM flask. Well, he ended up dropping the whole spatula in (About 2g worth. He wasn't worried at first, about 10 minutes later it started bubbling, and they got bigger and bigger and bigger ... At this point he nearly shit his pants. There was a huge stream of gas shooting out of the top of the flask, luckily it was a widemouth flask and vapors we're trapped. He feels lucky on this part. He quickly grabbed some oven mitts, as at this point is was way, way, way too hot to touch, and put it in a bucket and covered it with a linen as to not trap the vapors but contain spittle that had started working its way up the inside edge of the glass. 20 minutes later, nothing but grey soup. This was SWIM's first and last incident as far as he is concerned. Now you know why SWIM is so overly cautious. Bee good. Bee cool. Bee safe.

PSS. Yes, SWIM was wearing the proper safety attire, safety glasses etc ... Needless to say, now, nothing more than SWIM is going to use at that moment ever leaves it's storage container.


"We can't solve problems by using the same kind of thinking we used when we created them."

[Osmium]

I can't believe this.
You can do that reaction easily in a fucking 2L flask, IF YOU USE THICK AL. In a 12L flask you could make 500g runs without a problem. Use the fucking search engine. All your questions have been answered before. Repeatedly.
I'm not fat just horizontally disproportionate.

[overclock]

Yes Os, I know UTFSE. SWIM normally does but his time to sleep and dream is limited and needed answers within a context of time. He beelieves his answers have been sufficiently answered to sleep tight ...

Thanks,

Peace.
-OC
"We can't solve problems by using the same kind of thinking we used when we created them."

[Beaker]

I can't believe this.
You can do that reaction easily in a fucking 2L flask, IF YOU USE THICK AL. In a 12L flask you could make 500g runs without a problem. Use the fucking search engine. All your questions have been answered before. Repeatedly.

Here it is again

In a 5L two-necked flask equipped with an overhead stirrer and a reflux condenser with ice-water circulating through it was placed 2L MeOH. .5g HgCl2 was added and stirring commenced. Once the HgCl2 was completely dissolved, 120g of Al sheet, cut into 1/2" squares was added and stirred vigorously for 30min. 700g 40% Aq. MeNH2 followed by 534g of MDP2P were added in single portions, and the funnel was rinsed with 200mL of MeOH. The reaction was briefly heated to reflux temperature, the heat removed, and the resulting exothermic reaction cooled with a water bath(room temp water is OK, no ice needed) in order to maintain a light reflux(the reaction will run away otherwise). After approximately 1.5-2hrs, the exothermic reaction had subsided, the Al was mostly consumed, and TLC showed no ketone present in the rxn. The reaction can be worked up by any of the usual methods(repeated MeOH extractions of the sludge were used in this case). After A/B, distillation of the freebase, crystalization, and recrystalization from IPA, the yield of MDMA HCl(averaged over repeated runs) is approximately 450g, or 65%.

Also, just to give him his props, this procedure was based on Osmium's write-up on Rhodium's page and modified slightly over time.

Notes:

The Al was flashing from a major U.S. hardware store chain with an orange sign, sorry don't know the thickness. Watch out, as they sell another type of Al flashing that has a plastic coating and comes in the exact same packaging.

Ketone was simple distilled from modified performic, generally containing an unknown(5-15% ) amount of unreacted isosafrole due to shitty H2O2.

40% MeNH2 was made starting from hexamine camping fuel in a procedure similar to that covered in Chromic's writeup and elsewhere on this site.

[overclock]

SWIM gets what your saying. The main limiting factor in SWIMs dreams at the moment is stirring. SWIM doesn't like to ghetto rig, and he doubts magnetic stirring would be sufficient for what you have recommended. He has the glass connectors and such and teflon paddle but no overhead stirrer. It is next on his list but has not found a suitable one in his price range yet. Thanks for the mini writeup beaker, I'll bookmark it for SWIMs future reference.

Peace.
-OC
"We can't solve problems by using the same kind of thinking we used when we created them."

[Chromic]

Beaker, I'm honored to have my name mentioned in one of your posts! I really look up to the work you've done, and the knowledge you've contributed to the hive. Keep up the good work.  

[Osmium]

I repeatedly prepared at least the same weight or more of distilled and crystallized MDMA than ketone used. Add the ketone dropwise, not all at once.
I'm not fat just horizontally disproportionate.

[placebo]

An overhead stirrer is too easy to rig up, look on Rhodium's page.