MM's Al/HG Condenser H2O Temperature

[Diggity]

I thought that excess MethylAmine gets formed when the aq base is added to any existing al chips..

Filtering is a bitch, and a timely process, even more so on larger scales and will require a huge buchner. Swim has noticed that letting the post rxn contents stir for a good 24 hours will leave virtually no al chips. If your pressed for time, deal with the smell.. if not, then let it sit, stirring. Yields have been consistant. 23ml ketone -> 20-21g of clean product. When scaled up alot, it's almost necessary to let it stir for a long while to allow cooling. Picking up a 5L or 12L flask when hot could turn you into a very a sad bee.. heh, just the thought makes me wanna cry. Let that shit cool for a LONG while.. why risk it at that scale. Not to mention.. letting it stir for excessive amounts of time may increase yield also. 

The shitty thing about this is the amounts of non polar needed to collect the freebase.. I don't understand why so much is needed. 700ml per 20g of product is so much.. Why can't one just use 200ml's and let it stir for another 24hrs, ensuring all the freebase gets in the non polar? Why is so much used!
& I'm, somethin of a phenom, 1 puff of da cron, I'm un-stopable.   
 

[lab_bitch]

Why can't one just use 200ml's and let it stir for another 24hrs, ensuring all the freebase gets in the non polar?

You could let it sit for a million years, but there is an equilibrium partition coefficient for the MDMA freebase b/t the MeOH/H2O and the toluene.  In other words, you can only extract a certain percentage of the freebase with one extraction.  To extract more, you must use fresh toluene and perform a second and third, ect.  The reason that so much toluene is required, is that the freebase is pretty soluble in the aqueous layer due to the presence of the methanol.  If you follow my workup procedure, there will be no methanol left, and the freebase will form a separate layer that can be removed with a sep funnel.  Just to scavenge up any stray freebase, I go ahead and extract the aqueous layer with ~100 mL toluene once or twice.

[Diggity]

Lab bitch..

Swim never extracts more than once. He always adds all his freebase at once, stirs for 10 minutes, then extracts and always gets back the desired amount of product. I never really undertstood the logic in doing separate extractions/additions of non polar.. either way it's all gonna end up in there anyway.. why bother fucking around with extra steps. Every single time 23ml of ketone brings back 20-21g of product. I doubt he will see any difference if he collects his freebase in 1 step or 20.

f you follow my workup procedure, there will be no methanol left, and the freebase will form a separate layer that can be removed with a sep funnel.

Please! Direct to me this method!    I know one can distill the freebase oil out of the meoh, but thats not time efficient by any means. Without a rotovap, swim kinda sucks.. Next toy on the list  
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[goiterjoe]

Have you actually filtered off the sludge w/o basifying first? 

What, you think I'm going to suggest something without trying it?  When you basify your sludge wholesale, that's hydrogen gas being emitted, not methylamine.  The mix also heats up to around 50C and takes a while to cool back down.  The sludge is messy in a separatory funnel, and toluene takes forever to separate out of it.  That 5 minutes spent filtering the aluminum will save you over an hour of workup time without. 

as far as ratios, my last one was 27g ketone, 20ml water, 35g nitromethane, and 33g aluminum.  I liked to raise my nitromethane levels over the suggested amount.  I switched between using 2L and 3L flasks, depending on which one is not being used at the time for other things.
All paths are the same: they lead nowhere

[Diggity]

Joiter.. have you ever had sucess using sheet with nitro? Just curious why more people don't talk about using sheet or thicker al. I would guess if you are just animating 27g of ketone, you wouldn't want to spend all day doing it.. I understand that completely.. im just wondering why it's not mentioned more..

You make alot of sense though.. I know of the time you speek of fucking around with emulsion and other bullshit. Swim has filtered b4 and was very happy with the end results.. it just became impractical as he doesn't have a buchner that can handle the amount of sludge he is filtering these days. Yearning to be able to soon say "fuck foil" even though it has treated many well.. 
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[goiterjoe]

I've never bothered with sheet aluminum, and doubt I ever will.  as of right now, I'm retired, and probably will be for several years.  I do have thoughts about getting back in the game again once sassafras oil gets banned in the US though.  At that time, I'll be looking to do some massive scaling up, and will be using methylamine instead of nitromethane.  The convenience of nitromethane makes it seem like a better option for small scale operations, but it's not worth messing with if you want to cook several hundred grams as a time.  That 3L flask you are currently maxing out to cook 25g can handle reducing 100g ketone using methylamine.
All paths are the same: they lead nowhere

[Diggity]

Sheeeeit!    You should be able to reduce more than that in a 3L    Alot more! Just figure.. in a 2L flask, using AL 10x as thick, should be able produce 10x as much as MM's.. thats 230g's of mdp2p reduced in a 2L right there.
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[goiterjoe]

I'm planning on going PIHKAL #109, scaled up of course.  Hell, I might even see about making some of Osmium's modifications depending on the journals he referenced.
All paths are the same: they lead nowhere

[Osmium]

Swim never extracts more than once. He always adds all his freebase at once, stirs for 10 minutes, then extracts and always gets back the desired amount of product. I never really undertstood the logic in doing separate extractions/additions of non polar.. either way it's all gonna end up in there anyway.. why bother fucking around with extra steps. Every single time 23ml of ketone brings back 20-21g of product. I doubt he will see any difference if he collects his freebase in 1 step or 20.

*Banging head against the (concrete, not dryboard!) wall*

Someone tell me he didn't say that...
You might not understand why extractions have to be repeated, but others sure do! So when the writeup says extract 3 times then fucking do it!!! FYI, you poured several grams of perfectly good honey down the drain every time you were too lazy to repeat the extraction. Great job, I hope saving a few minutes of work was worth it.
I don't get it why people take shortcuts like this, wasting their precious end product after they spent days of hard work and expensive chems to prepare their precursors.
I'm not fat just horizontally disproportionate.

[Osmium]

> You should be able to reduce more than that in a 3L. Alot
> more! Just figure.. in a 2L flask, using AL 10x as thick,
> should be able produce 10x as much as MM's.. thats 230g's
> of mdp2p reduced in a 2L right there.

This will not work. You can only aminate 200g ketone in such a flask when you have methylamine. The reduction of the nitromethane needs so much Al that your flask will be filled with clay-like, almost solid chunk of sludge when done.
I'm not fat just horizontally disproportionate.

[Diggity]

Osmium.. if you used 23ml's of ketone, and got back 20-21g of product consistantly, how/why/amImissingSomethingHere am I going to get more product back!! Ok.. so what your saying is you suspect my yields to be 100% g/g.. because thats what im reading.

If swim adds all his non polar, like he does every other time, the past 100 or so times, and always gets back what the synth details.. sometimes more! (rarely, happened twice or so)

I just don't see the big deal, if either way you are putting in 700ml's of non polar.. then either way, ahhh whatever. With strong stirring, the shit migrates all at once instead of in parts.. Im sorry for not seeing the logic there. It just doesnt make sense to me.. It's been done both ways. Swim started off doing the 2 extractions.. then said fuckit one day and did it all in one.. low and behold, no difference whatsoever, except the time and energy spent inhaling toulene.

imho, if swim saves a few brain cells from not inhaling/being exposed to the shit an extra few minutes, then it was well worth the 1/2 - 1/4 gram that may have made it's way down the drain.

Swim will try this again.. and chart results. I got a cool grand that says the results won't be any more different, given the same amount of time spent stirring both ways.
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[Osmium]

Yeah whatever.
All these chemists who been doing this for well over a hundred years are idiots since Diggity says so.

> Osmium.. if you used 23ml's of ketone, and got back 20-
> 21g of product consistantly, how/why/amImissingSomethingHere
> am I going to get more product back!!
 
For your information: 23ml of ketone are 27.6g. 100% yield of final solidified honey would be about 30g. Your yield is 20-21g which happen to be about 66% (again, just estimated). So where did the rest go?

> it was well worth the 1/2 - 1/4 gram that may have made
> it's way down the drain.

Make that 2-4g, proportionally more for bigger reactions.
Sigh. Oh well. It's your yield, your money and your time you are wasting, not mine. If you can live with these losses, fine. I couldn't
I'm not fat just horizontally disproportionate.

[Diggity]

hrmm, I feel tiny right now. swim will give the 2 part extraction another chance, being that it was so long ago that swim used it, yields may have increased alot now that different equipment/technique is being used.. ie. stirrer, bar.

Shit, I'll feel like such an ass if your right. heh, it just doesn't make sense in my head.. thats all.
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[goiterjoe]

we don't do 3 extractions just cause we feel like it.  Your yields will go up.
All paths are the same: they lead nowhere

[lab_bitch]

[Diggity]

The rate of products formed (condensing/evaporating) - equilibrium?

If not, then fuck you still.

Os, You were right, as I suspected.

Swim was very precise with all measurements, and rxn was done 3x, only results for 2 in so far.

In a 5L rb

68.75g of al
1875ml of meoh
1g hg

50 ml of nitro, (20 ml added first, then ketone)
57.5 ml of mdp2p

rxn went smooth in all 3 instances, sat for a few extra hours,

Basified cold using 655g naoh in 1750 h2o

in the first scenario swim was sure to dump in all non polar 1750ml's at once
proved to yield after 2 tone washes was 48.5g, expected 52

In the second scenario no variables were changed except the non polar was added in 2 portions, 900, then 850..  yield after 3 tone washes.. 52.5, approx 4 gram difference.    POINT PROVEN.. BUT! shoulda been more.

Swim has yet to basify the 3rd rxn as exaust settled in, but will try again with 3 extraction.. the first being the 900, the second, 400, then 450. I can't possibly see the yield go up much more, and was pretty shocked at the first one being as low as it was.. usually it returns 20-21g per 23ml, when done at scale.. being done at 2.5 scale shouldn't of made a difference, although there was alot more room in the 5L than expected.. should of done at 3x scale in a 5L..

Could the extra head room in the flask of effected yield?? 

Hey bitch ass, it appears the equilibrium was shifted due to the excess head room? no? 
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[Diggity]

HAHA! Os, Os, you called it, 54.2 g total after 3 tone washes, 99%+ purity! How do I know? Not a scent to it and not a morsel sticks to the bag!!    Thank you.

I almost expected that. Well, honestly, I didn't expect more than a gram more than the last, and low and behold, 1.75 g more doing all 3 extractions! Thats equivilant to 135 sand dollars!    AND YES, it was worth the extra 10 minutes it took.    Thank you again.      
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[scram]

Yeah, what is this sticking to the bag mean. Someone was trying to tell me that pure mdma will not stick to a bag, something about polarity. But I had passed this as stupid raver kid nonsense.

[Diggity]

Probably oil's from the non polar it was once in..

Give it a tone wash, or two, ANHYDROUS, and you will be happier, but not much happier, I mean, it all depends on how happy pure drugs make you. Lately, drugs arent making me happy.. it's mainly cuz Im not doing them.
& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

[Osmium]

> what is this sticking to the bag mean. Someone was trying to tell
> me that pure mdma will not stick to a bag, something about
> polarity. But I had passed this as stupid raver kid nonsense

I think that person was talking about electrostatic charges (the comb atracts hair phenomenon). I made MDMA that did stick to the bag, and also some that didn't. MDMA gassed in IPA/acetone showed this behavior, when you try to fill a baggy with it the crystals will start flying since they seem to get charged easily, and they also stick to the bag and resist to fall off.
MDMA crystallized with IPA/aq.HCl/Et2O or by gassing an Et2O solution didn't show this behavior at all. I don't know what the reason for this is, I can only assume that the latter contained some water of crystallization or at least a conductive water film on the crystal surface while the former didn't.

The MDMA was very pure in both cases, and that this sticking to bag phenomenon indeed exists, but it's not possible to use it to decide about purity, since too many other factors play a role in the occurence of electrostatic charges. Relative humidity of the air, crystal size, presence or absense of impurities and water, and even what kind of clothes you wear and what the floor you walk on is made of might all contribute to it.
I'm not fat just horizontally disproportionate.