MM's Al/HG Condenser H2O Temperature

[Bubbleplate]

SWIM has well water that is a constant 11 C. Is 11 C. cold enough to run through the Allihn Condenser for the MM Al/Hg Reduction?
SWIM has used this setup for other refluxes, etc. and water always seemed cold enough.
If they drive God from the earth, we shall shelter Him underground - Dostoevsky

[pickler]

You want your water as cold as possible, that's why it calls for ice. Once you run the synth, you'll understand why you need ice cold water.
I went into the business for the money, and the art grew out of it.-Charlie Chaplin

[weedar]

A bucket filled with ice and then filled with water?
Throwing in more ice if needed.

Weedar
Save the Temporary Couch! And whales.

[Chromic]

Cold water is fine if you don't recirculate... the reason MM calls for ice is because he uses a bucket to recirculate water and it'll eventually heat up the water.

[Diggity]

I disagree chromic. YOU WANT THAT SHIT ICE COLD!!! Trust that. Even with (2) .99c bags of ice, one may end up with a little reflux escaping.

The amount of ice needed will also reflect how fast the addition is done. Swim likes a fast addition, so he uses HUGE bags of ice, freezing fucking cold. Even then, on occasion, he has to stop/slow the addition as reflux is noted creeping up the condensor.  Cold water from your faucet will not cur it, unless you wanna spend a good hour and a half adding your goodies.
& I'm, somethin of a phenom, 1 puff of da cron, I'm un-stopable.   
 

[Bubbleplate]

of H2O re-circulating through Ice Bucket? If it isn't in the 4 or 5 C. range, then I think 10 or 11 well water and an 8 Bulb Allihn may be OK....
If they drive God from the earth, we shall shelter Him underground - Dostoevsky

[Osmium]

If your reaction is running so hot that it stinks up your room then you should slow down somewhat. Can't hurt to cool the flask either in that case.

But you are missing the point, you guys should reduce the MeNH2 separately from the ketone, suddenly th reaction will be MUCH more controllable and yields will usually go up too.
Even if that way is somewhat wasteful on the nitromethane, which reagent is cheaper and easier to obtain? MDP2P or nitromethane???
So there. Maximise your yields dammit!
I'm not fat just horizontally disproportionate.

[goiterjoe]

you guys should really consider slowing down your addition rate.  Cold water with no ice works just fine if you use a lot of it for recirculation and use a reasonable addition rate.

All paths are the same: they lead nowhere

[Bubbleplate]

separately from the ketone? Are you saying add the Nitro first, or actually do a separate reduction of the Nitro with Al/Hg, isolate and then use the Methylamine directly with Ketone???
If they drive God from the earth, we shall shelter Him underground - Dostoevsky

[wyndowlicker]

Swiw would like to add a few words here.!A 1 pound bag of ice cuts it for swiw.There should bee no reflux escaping at all if you dont do you addition in 4 minutes.Swiw makes sure his addition is no faster than 5/8th the rate of reflux returning to the flask.Thats about 2 drops per second.Startwith 1 till it gets going.Swiw finds if the addition is too fast Your sludge thickens and stirring is inhibited.Leading to a need for addition of MeOH.Perhaps with a 5-600MM reflux column can handel those quick additions,But swiw doesnt feel safe going that fast.Why rush it 30 minutes.Swiw never broke the rreflux rate during addition and had terrable yields.Wont bee doing that again.
Counting starts by candlelight all are dim ,but one is bright.-GD

[Bubbleplate]

SWIM decided to try the Ice Bucket/Recirculation to "bee on the safe side". 8 lbs. ice in 5 gallon bucket. Halfway through the MM Al/Hg ketone addition, all the ice had melted. SWIM decided to switch over to straight well water from faucet, just as reaction started to really "take off". Turns out methanol vapors never got much past the 3rd bulb of an 8 bulb Condenser, and reflux was "pouring like rain" from bottom. Looks like 12 C. H2O is just fine with 2K ml Flask and 8 bulb Allihn.
BTW, the actual reaction temperature peaked at 71 C., and stood at 65 C. throughout most of reaction. Took a long time to come down to 50 C.

If they drive God from the earth, we shall shelter Him underground - Dostoevsky

[lab_bitch]

I was under the impression that adding your reactants faster gave better yields.  Personally, I have run the reaction with PURE ketone and can never get close to Baalchemist's 30g MDMA/30g ketone.  Mabey my aluminum sucks.  I usually add the reactants in about 15 minutes and get 20g MDMA/30g ketone.

[goiterjoe]

you can get gram for gram yields by adding your nitro first as fast as you can, letting it settle back down some, and then dump your ketone in wholesale.  27g ketone in, 27g crystal out.
All paths are the same: they lead nowhere

[lab_bitch]

Damn!  I'll give it a shot.  How much HgCl2 to you use per gram aluminum?

[Diggity]

I was under the impression that adding your reactants faster gave better yields.

I agree, it's true, although, joe has me very excited over here.. Gram for gram? Eye for eye? Joe? Say it again man!? Is it really so?

Swim has added 3/4 his nitro first before and hasn't been granted g/g access.. Im sure 3/4 or 4/4 wouldn't make a world of difference at that point, though he will try again. G/G on a a foil rxn would be very nice!    

Shal swing all, then all.. interested..    I also have a headache.
& I'm, somethin of a phenom, 1 puff of da cron, I'm un-stopable.   
 

[goiterjoe]

yes, gram for gram can be seen from a nitromethane reduction if the nitromethane is allowed to reduce first to methylamine.  The reaction should have a small amount of water added to it, and that will make it run a LOT hotter than if it is anhydrous.  it will also make a serious difference in yields.  Another yield inhibitor is ketone purity.  If you're not getting clean fractional separation when you distill your ketone, then your yeilds will suffer as well.  The last thing that will help is the basification process.  Don't basify the reaction wholesale, but instead filter out the aluminum sludge and back wash it with some methanol and basify the extracts.  It is a lot cleaner and easier, and can make it a lot easier to get good NP separation.
All paths are the same: they lead nowhere

[Protium]

I was under the impression that adding your reactants faster gave better yields.

While in many cases this is do-able, just dumping in the ketone wholesale really is not the way to go, and will most often in larger reactions stink up your workspace.  The devil is in the timing, slower titration in the correct timeframe would be higher yeilding than a wholesale dump, as it is prefferable to have a large excess of the methylamine to the ketone, however many bee's who set their addition funnels to a slow drip rate and allow the addition to continue after the amalgum is spent, wind up with a lot of unreacted ketone in the mix and the yeild is shit.  It's all about the thickness of the aluminum and the timing of the amalgum, thicker aluminum and slow titration is ultimately higher yeilding.  However, slower drip rates are not always an option for those who opt to use aluminum foil.  This is balanced somewhat, however, by a pre-addition of the nitromethane to facilitate the excess, although I have found as a general rule slower additions when properly timed are considerably higher yeilding, and easier to control.

Moral to the story : timing is everthing
Pr(+)tium

[lab_bitch]

goiterjoe:  How much water is "a small amount"?  How much HgCl2 do you use per gram of aluminum?  What is the scale of your reaction?

Have you actually filtered off the sludge w/o basifying first?  It is a BITCH!  By basifying the reaction, you are converting the aluminum hydroxide/methoxide into NaAl(OH)4 which becomes a small black blob on the bottom of the flask.  Filtering takes about 5 minutes.  You must add the base correctly, though, or you will not get this awesome precipitation.  Here is how I do it:

After the rxn is done (it is not necessay to let is cool down first), add exactly 500g of 25% NaOH to the rxn while stirring the reaction at maximum speed.  This addition should take between one and two minutes.  You don't need to drip it in, but you don't want to dump it in all at once or your rxn mixture will become the consistancy of clay and will require lots of extra base/solvent to salvage.  After the rxn stirs for a few minutes, the fine particles of aluminum will begin to coagulate while a good deal of MeAm gas is evolved.  One the gas stops coming off and making the aluminum float, give the flask a good shake and all of the aluminum will sink to the bottom, leaving crystal clear solvent on top.  If you let is sit overnight at this point without stirring, the aluminum will collect into a golf ball sized black blob that is stuck to the bottom of the flask and you can simply decant the solvent without even having to filter it.  Then just strip off the methanol and perform an A/B, distill the freebase, and gas.  The above method is for 30g ketone, 24g MeNO2, and 33.5g Al.  If your numbers are different, you may require a different amount of base.

[lab_bitch]

I know that Al thickness is very important in this rxn, but does it matter how small the Al squares are cut?  Because I have better things to do with my time than cut up aluminum, I bought a paper shredder that cuts the foil into pieces about 1x1/2 cm.  I then grind them in a paper cutter.  I use Reynold's Heavy Duty, by the way.  Would this make a difference as opposed to cutting the pieces bigger (1 inch squares)?  Also, does anyone have experience using aluminum pie pans or other thicker aluminum with this particular reaction?

[Rhodium]

If you perform the reaction as in Pihkal #109, but before filtering you add X milliliter 25% NaOH for every X gram of aluminum used from the beginning and then stir the reaction mixture for 30 minutes before you filter it all through Celite (common "dirt cheap"  diatomaceous earth), then the filtering will take at most 5 min at the same scale as Shulgin's.

[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.

[humidbeing]

You're cool osmium.
CG I miss you sweety, I really do.

[goiterjoe]

don't you people package with wax paper like normal people?  I couldn't imagine dumping powder into a baggie.
All paths are the same: they lead nowhere

[Rhodium]

Why are you dumping MDMA.HCl into "baggies", when it belongs in gelatin capsules? With a drug like meth where the dosage is entirely random, I can understand the ziplock distribution, but not when it comes to MDMA, where "one dose fits all". How can you be sure that people further down the line will re-package it into proper doses? If anyone has a good scale and knowledge of a correct dose, it should be the chemist himself.

[Osmium]

> Why are you dumping MDMA.HCl into "baggies", when it belongs in gelatin capsules?

Because I stored some stuff that way. It's much less suspicious to show up with a small baggy of white powder at work and weight it on one of the scales there than handling empty caps in the weighting room.
It's also possible that (many moons ago, when I was still young and stupid) used a baggy to ship stuff from A to B, I really can't remember the details.

I'm not fat just horizontally disproportionate.

[goiterjoe]

It doesn't take much effort for the person to skim off the top of the capsules after you took the effort to put them together.  It pisses me off that people will do this, but nevertheless it happens.  I always package MDMA in capsules if someone else was getting it, but I always carried speed in wax paper.  If I was going to split the MDMA among a small group of friends who like to snort things, I would package it up in wax paper and split it out later.
All paths are the same: they lead nowhere

[wyndowlicker]

Here is my observations.people will cut 12 pill out of a gram.Make it so noone rolls well.Pressies are what everone wants because they no no better.Clubbers dont like pure MDMA they like it dirty.With "Heroin"or speedy.The few that I actually think might understand that H isnt in anyones pills and why.Usually dont believe me.Or care for that matter.As long as they get what they want.Alright you want it speedy how would a 60% caff. cut treat you?Good?Have a nice day!Most are like I wanna go dance on it not Fuck,or bee so fucked up I cant go out.Gotta fix that. Ever tell anyone that dirty pill has too much HCL or mercury in it?The look is priceless.Just dont do it around close friends or they night think your crazy or worse .Fair warning!
You can tell the queen of diamonds,by the way that she shines.-GD

[Bwiti]

"But you are missing the point, you guys should reduce the MeNH2 separately from the ketone, suddenly th reaction will be MUCH more controllable and yields will usually go up too."

  Yes, this way additions can be done quicker, and it can be done under pressure to increase yield without getting out of control. Btw, by under pressure, I mean rigging the reaction vessel to a devise similar to an RP/I push-pull. Peace!

Love my country, fear my government.

[Rhodium]

What kind of pressure would result if the Al/Hg reductive amination was performed in a closed pressure vessel? If completely gas tight, no methylamine would escape, and the reaction would be forced towards product amine, as MDMA takes way less space than methylamine + ketone + hydrogen. The increased pressure would make the reaction run even hotter, so the pressure vessel would need to be properly dimensioned.

[Barium]

Rhodium:

I found something about just that a while ago. Reductive alkylations with P2P, MeNH2 or EtNH2, Al(Hg) in Et2O. If I remember correctly the pressure increase wasn´t too extreme. I´ll dig it up.
Catalytic hydrogenation freak

[lab_bitch]

If you use nitro as an amine source, you'd better have a hell of a heat exchanger.