Purification of MDMA by recrystallisation

[HOOH]

Why not distillation?

can you explain what you mean by "mddm is a known inhibitor of mdma"? and simply quote the part of that text which validates it.
People here have a habit of claiming something then dropping a book on the desk of anyone who asks for clarity. Reading 100 paragraphs to find 1 (which may or may not even be there) is not an efficient way to back up claims.

As for distillation, their melting points are too similar.
As for the MDDMA being an inhibitor, I THINK that OP means that MDDMA would partly displace the MDMA molecule out of the neuron, but since MDDMA is much weaker, it's weakly akin to an antagonist.

 

[vecktor]

@vecktor thanks so much for replying! I got a few questions:


Yeah I was thinking of doing it 3 times, each time recrystallising half and chucking the rest. Fingers crossed that's enough to get rid of the impurity if it can be done via this method

go from boiling to ice cold let it stand and collect all the crystals, Rule 1, don't throw anything away. the impurities end up in the mother liquor. Also don't even throw the mother liquor away until you have what you want. Best practice is to allow the mother liquor to evaporate and allow the stuff you don't want to crystallize too.
The other good practice, but often tricky to do simply, is to filter the hot solution whilst it is still hot to remove any insoluble material

If you want to recrystallize again then recrystallize all the crystals from the previous crystallization. guessing half or whatever is a waste of time your total product will get smaller and smaller without trying too hard.

I would guess that MDDMA is only present at 10% or less and a single crystallization would remove it. If it is dimers then a single re-crystallization will remove it.

look up melting point determination, it is very simple with a tube and thermometer in a test tube of oil and that gives you a check of purity, be aware the literature says that the hydrochloride exists as multiple hydrated forms so what you are looking for is the increase in mp to stop.

from Pihkal: Only the anhydrous form has a sharp mp; the published reports describe all possible one degree melting point values over the range from 148-153 ° C. The variously hydrated polymorphs have distinct infrared spectra, but have broad mps that depend on the rate of heating.

So 99% IPA and don't worry about drying. Cool, that's nice and straight forward

Yeah that comment came from the bluelight post. Looked authoritative but I wasn't in a position to judge haha

Right, so just poor the near boiling ipa into the 'MDMA' conical flask? I guess I've just got to do that carefully

or put cold IPA in and heat it in the conical flask with the powder.

Right. To room temperature, or after that to fridge then freezer?

And is there value in adding the freezer cooled anhydrous acetone to the mix to help the MDMA crystallise out?

no acetone, you are not trying to crash out everything from solution you are trying to only crystalise the saturated component.
Anhydrous acetone is a bit of a myth most drying agents make diacetone alcohol from two acetone molecules and then this forms mesityl oxide. acetone so acetone plus drying agent is dry but impure.

One big worry I have, because I want to discard half each time, is how to judge when that amount has crystallised. If I just leave it the impurities will crystallise out as well. At the moment all I've got is eyeballing it. But visually I don't know how good my guess is going to be. Any ideas?

Thanks, I'm going to give it my best shot. I guess some of my questions might be a bit dumb but I appreciate that if this is worth doing then only if done right.

I was thinking of getting a hot plate/stirrer. I know there's concerns about heating up IPA but I'm assuming the quantities here are not too risking. Would the magnetic stirrer in the IPA be useful while heating or unnecessary?

you can heat it with a hot air gun, hold the flask with a glove and swirl it when you heat it.

 

[vecktor]

As for distillation, their melting points are too similar.
As for the MDDMA being an inhibitor, I THINK that OP means that MDDMA would partly displace the MDMA molecule out of the neuron, but since MDDMA is much weaker, it's weakly akin to an antagonist.

distillation separates things as vapor (a gas) exploiting the difference in boiling point. the melting point of the material does not matter

distillation to separate the dimethylamino compound from the methylamino compound is extremely tricky because the boiling points are going to be close especially as this distillation has to be done under vacuum.

 

[HOOH]

distillation separates things as vapor (a gas). the melting point does not matter

My bad, I meant to say boiling points.
But alas, my point doesn't change, for their boiling points are too similar.

 

[ThreePointCircle]

The other good practice, but often tricky to do simply, is to filter the hot solution whilst it is still hot to remove any insoluble material

Is that not just a case of when the mdma is dissolved in the hot IPA, poor the whole lot in a funnel with filter paper in it, into another beaker?

If you want to recrystallize again then recrystallize all the crystals from the previous crystallization. guessing half or whatever is a waste of time your total product will get smaller and smaller without trying too hard.

Oh right. I was a bit paranoid about recrystallising the impurities. So are you saying I'm unlikely to crystallise more than, say 85% of the original anyway, so I don't have to guess at it?

I would guess that MDDMA is only present at 10% or less and a single crystallization would remove it. If it is dimers then a single re-crystallization will remove it.

So perhaps doing it twice to make sure is enough?

look up melting point determination

Ok, will do

or put cold IPA in and heat it in the conical flask with the powder.

Ok. So add a bit, warm it up, and a bit more, warm it back up, repeat till it dissolves?

no acetone, you are not trying to crash out everything from solution you are trying to only crystalise the saturated component.
Anhydrous acetone is a bit of a myth most drying agents make diacetone alcohol from two acetone molecules and then this forms mesityl oxide. acetone so acetone plus drying agent is dry but impure.

Right. That's funny, amazing how stuff is said and repeated without it being right.

you can heat it with a hot air gun,

Oh that's easy as I have a decent one. Set to what, like 100 deg C? Only used one for soldering before

 

[vecktor]

Is that not just a case of when the mdma is dissolved in the hot IPA, poor the whole lot in a funnel with filter paper in it, into another beaker?

yes but it has to stay hot and when it gets into the funnel it will cool fast due to evaporation and try and crystalise in the funnel and on the paper, You'll see.

Oh right. I was a bit paranoid about recrystallising the impurities. So are you saying I'm unlikely to crystallise more than, say 85% of the original anyway, so I don't have to guess at it?Only the anhydrous form has a sharp mp; the published reports describe all possible one degree melting point values over the range from 148-153 ° C. The variously hydrated polymorphs have distinct infrared spectra, but have broad mps that depend on the rate of heating.

85% you would be lucky! think more around 75% max recovery from one crystalisation even at ice cold.

So perhaps doing it twice to make sure is enough?

would have thought so

Ok, will do

Ok. So add a bit, warm it up, and a bit more, warm it back up, repeat till it dissolves?

yes but be aware there might be some insolubles if the material is impure which will never dissove no matter how much solvent you use

Right. That's funny, amazing how stuff is said and repeated without it being right.

Oh that's easy as I have a decent one. Set to what, like 100 deg C? Only used one for soldering before

IPA boils at 82 degrees so 100 is fine. using a conical flask is safer than a beaker because you can see the vapor creep up the flask, the upper flask acts like a temporary reflux condenser. obviously heat the flask or the beaker not the liquid directly and remember you are heating something flammable! so don't let lots of vapor get into the heat gun. (the elements are hot enough to light some solvents)

 

[ThreePointCircle]

yes but it has to stay hot and when it gets into the funnel it will cool fast due to evaporation and try and crystalise in the funnel and on the paper, You'll see.

Should I pre-warm the funnel with the air gun to help with this? Is it worth doing given the difficulty?

85% you would be lucky! think more around 75% max recovery from one crystalisation even at ice cold.

Ah, I see. So as long as I'm diligent this should work fine then without the guess work.

yes but be aware there might be some insolubles if the material is impure which will never dissove no matter how much solvent you use

Right, so perhaps be tolerant of a few little bits?

IPA boils at 82 degrees so 100 is fine. using a conical flask is safer than a beaker because you can see the vapor creep up the flask, the upper flask acts like a temporary reflux condenser. obviously heat the flask or the beaker not the liquid directly and remember you are heating something flammable! so don't let lots of vapor get into the heat gun. (the elements are hot enough to light some solvents)

I saw in the original plan they suggested laying aluminium foil over the top while heating the ipa. Is that worth doing or just rely on the conical flask and observing the vapor creep?

 

[G_Chem]

Most illict MDMA is not synthesized directly from methylamine, rather the methylamine is produced via the reduction of the widely available nitromethane with Al(Hg).

Wrong. Nitromethane is only used in small batches with hobby chemists, the glassware size required to do an amination with nitromethane is too large to make it worth it.

Next most MDMA these days is made via Pt hydrogenation (as has been shown with proper articles on the other thread) and because of that again won’t be reduced with nitro but methylamine.

I’m beginning to see your someone with some book knowledge if chemistry, but nothing much more than that.

If you’d like to hang in this discussion I suggest you do your research on MDMA synthesis trends over the years before jumping in again.

Plenty of chemists make their own methylamine, honestly it’s easier to synthesize bulk methylamine than it is to even acquire bulk nitromethane.

The most common route most use to get there is either hexamine or paraformaldehyde, both of which can have both ammonium and dimethylamine as potential impurities.

-GC

 

[HOOH]

Next most MDMA these days is made via Pt hydrogenation (as has been shown with proper articles on the other thread) and because of that again won’t be reduced with nitro but methylamine.

Do you have any sources for this? Because I highly doubt the existence of somekind of an MDMA-superlab, which have access to Pt hydrogenation methods. As far as I know, most MDMA is made exactly by these "hobby chemists". This is also implied by the variation of quality and appearance found in street MDMA.

 

[Ambien Powered Rabbit]

To the OP: can you explain what you mean by "mddm is a known inhibitor of mdma"?

I THINK that OP means that MDDMA.....

yes I can make my own assumptions about what the OP may have meant. something like "people will see a paper about inhibitors, substrates, binding affinities and they will not question what I am claiming". maybe I am wrong but I would like to hear it from the op.

really should be a breeze for someone who understands all those complicated sciencebook words

 

[ThreePointCircle]

So step one is done is on its way to completion. I've got the beaker currently cooling in the fridge and recrystallisation has begun. Things I noted:

• I don't know if it had any value but I ground the product a bit with mortar and pestle. The crystals were initially yellowish but as I ground them the became whiter. Don't know if that is of interest or not.
• I had to set my heat gun up fairly high - 250 deg C ish. Maybe that was because it is designed for electronics I don't know but it was taking forever at a lower temp. It wasn't quick at that temp, seemed just right
• It took a lot less IPA than I thought, perhaps 3ml for 3g of mdma when heated
• I did filter, and as it was filtering I heated the funnel from below using the heat gun. It didn't look like much if any recrystallisation happened in the funnel. I bit of liquid was left in the funnel as it was taking an age to drain towards the end so I made a decision and left it out
• Recrystallisation began at room temp, beaker covered in foil. I've now transferred to the fridge.
• The liquid has a yellowish tint

 

[ThreePointCircle]

Ok slight problem. Just checked back in the fridge and all of the IPA has pretty much disappeared and all the product has crashed out!

Think I'll try again with more IPA, won't bother with the filter, and do room temperature so it doesn't crash out

 

[ThreePointCircle]

Sorry for the delay. I did have a go. The product looked cleaner, and perhaps was a little better in the come up but clamped down as usual.

So either the method doesn't get rid of the impurity (assuming it exists) or I botched it. My only thought about botching it was that the recrystallisations I did were quite quick (lets say approx. 1 hr). Is that too quick? Did I rush it. I did hugely reduce the amount of product, although I've kept the 'waste', so I assumed it would still do the separation but does that speed of recrystallisation risk all the products crystallising out simultaneously, rather than the more concentrated one first?

I found the balance between recrystallising and not seemed quite delicate. First go where I just added enough IPA, recrystallised within minutes after cooling. I started again when that happened. The next time I added a lot of IPA and then it didn't recrystallise after 2 hrs so I heated the mixture to evaporate off some of the IPA to stimulate the process, but I don't know if that was a bad thing to do.

Basically I was over keen to try it that night. To get this right should it be much slower?

And if that wasn't the problem, was there anything else I could have done better, or should try?