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recrystallization of mdma

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hellowhatwhat

Greenlighter
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Jun 11, 2015
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So I have a g of mdma that is ground into a very fine powder,almost like a dust,and it looks like it would be very hard to work with in terms of weighing it,looks like it would stick to everything.
I have heard about spreading it on a plate and putting a bit of vodka over it to get it a bit more crystallized again?Anyone any experience with this?
 
if you don't want to remove impurities i don't see the point in recrystallisation. power is easier to handle than crystal. it can stick to a plastic baggies (those suck for most drugs anyway), but it doesn't stick to paper folds.

the typical solvent for recrystallisation would be isopropanol, but be aware that you're always going to end up with less product than you started with. some mdma is inevitably lost in the process.
 
Honestly I wouldnt bother. There is nothing better about bigger crystals and most people break them up in some fashion anyway prior to ingesting. Powder has a greater surface area and thus has a fast absorption rate making it "better" in terms of onset of action.
 
I think the most desirable solvents for MDMA recrystallization are either dichloromethane (DCM) or acetonitrile (ACN). Careful with the ACN though! It is metabolized to cyanide in vivo and will kill you if you take much product contaminated with ACN. Make sure to dry your crystals under a heat lamp thoroughly in any case. (And to wash the powder thorougly under vacuum filtration with an organic solvent before attempting recrystallization.)
 
IPA as solvent, Acetone to force the MDMA out of the IPA solution.
Crystallisation will require _several_ days
 
bla-ljus said:
IPA as solvent, Acetone to force the MDMA out of the IPA solution.
Crystallisation will require _several_ days
Click to expand...

^ this. if you want more info:

Put your dry MDMA HCl in a beaker and set it aside for later. Now in a separate beaker boil 10-15ml 99% IPA per 1g MDMA HCl in a beaker in a shallow oil bath with a stirbar on medium, it is best to use an excess of more IPA than you’ll really need in the beaker. Gently lay a sheet of aluminum foil over the top of the beaker, don’t wrap the aluminum foil over the beaker so it’s air-tight because that might create excess pressure within the beaker, the goal is to just lay a small sheet over the open beaker to keep moisture in the air from getting into the IPA since anhydrous IPA is hygroscopic. Once the IPA is hot/boiling then remove the sheet of aluminum foil and reduce the volume of IPA a little bit to azeotropically remove the ~1% H2O present in the IPA, then remove it from the hot oil bath and slowly pour it or use a pipette to add boiling IPA to the other beaker containing the MDMA HCl. This must be done quickly so that the dry IPA doesn’t absorb H2O from the moisture in the air. Be sure to add just enough IPA to dissolve the MDMA HCl, you want to use the absolute minimal amount of boiling IPA. Swirl the beaker around after adding IPA to the MDMA HCl, you may carefully put the MDMA/IPA beaker on the hotplate to warm it back up as the IPA will cool off when you remove it from the heat to add it to the MDMA HCl. If you decide to put the MDMA/IPA beaker on the hotplate then continue swirling it across the surface of the hotplate and be careful not to hold it there too long, just a few moments to warm it back up again. You want all (or like 99 percent) of the MDMA HCl to be dissolved then cover the beaker with aluminum foil to seal it, pinch the edges of the aluminum foil around the beaker to make it airtight. Now let the beaker with the IPA/MDMA slowly cool to room temperature on its own. Once it has reached room temperature or is cool enough to where it’s only warm to the touch, then add 4x volume of freezer-chilled anhydrous acetone in relation to the amount of IPA you used. This is to help lower solubility of the MDMA HCl in the IPA. You wait until the IPA cools off before adding the acetone otherwise the acetone would flash boil. Now carefully move it to the refrigerator, once it has reached the temperature of the refrigerator then move it to the freezer. The goal here is to cool it as slowly/gradually as possible to ensure slow crystal formation, you want to be as careful as possible and not agitate the solution as that will disturb crystal formation. After approximately 30 minutes in the freezer you’ll start to see precipitation, however you’ll want to keep it in the freezer for longer. Once it has been in the freezer for anywhere from 8-24 hours then carefully vacuum filter off the crystals over a #103 filter by barely holding the vacuum tube to the barb on the filter flask to apply a light vacuum. Wash the crystals with a small amount of freezer chilled dry acetone if necessary. Now spread the crystals out over a drying dish and let the crystals air-dry (or use a very low heat source like a heat lamp). Once dry then macerate the crystals to the finest powder possible to release any solvent that may be in the crystal matrix and allow them to air-dry (or with heat lamp) once more. You are now left with bright white and odorless MDMA HCl, you’re done!


or you can just do an acetone wash to clean the surface of the crystals. if it's a fine powder then there will be alot of surface area and the acetone wash will be the way to go because of less mechanical losses, it's alot easier and it's alot faster.

poopstation said:
just wash the pills/powder with cool acetone...MDMA HCl is only marginally soluble in acetone..

it's not the acetone that will cause the loss during the washes, it's the water content in the acetone. mdma hcl is fully soluble in water and there's always water in acetone. totally anhydrous acetone is quite hygroscopic so keeping it totally anhydrous for any length of time is challenging, luckily the water content is fairly little so losses are typically low especially if you do your best to dry out the acetone first. as recommended above you can use freezer-chilled acetone to help lower solubility even more.

as to whether the washes remove certain contaminants/impurities/etc well that just depends on their solubility and what contaminant specifically you're talking about. anything that isn't soluble in acetone will certainly not be removed.

the washes are great but they only clean the surface of the crystals, to get the impurities out of the crystal matrix you must recrystallize if you find that the acetone washes weren't enough. anhydrous IPA is a clear, easy choice for recrystallization solvent. then wash once more. you'd be amazed what the recrystallization solvent may pick up by what color it is after recrystallization. unreacted precursors (saf/isosaf/mdp2p) are your main contaminant as they have similar solubility to mdma freebase and follow through most typical work-ups that don't include an a/b.
Click to expand...
 
I would not get IPA involved at any point personally. I've just not had good results from it's application in either recrystallization to clean up or crystallizing for aesthetics. For cleaning I'd recommend ethanol/EtOAc and for slow crystallization, a methanol/ether or DCM system. I've been very happy with the results from methanol/ether, IME it tends to form beautiful prisms rather than chunks.
 
Find a solvent that MD dissolves into at a certain temp but solidifies (recrystallized) in solution at another (lower temp). This will cause MD crystal agrigation and a large chunk of MD will grow.

Vacuum filter. Perhaps repeat (if your solvent is 100% pure with no residue your purifying the product aka washing). This is a simple explanation the process is not something someone without basic chemistry skills/education should undertake.
 
poopstation: what do you think the advantage is of pushing the MDMA out of the IPA using Aceton over just using Acetone? Does it yield cleaner crystals?

Thanks in advance!
 
If it's racemic, which it most likely is, you will yield more like pebbles vs crystals

This thread is nearly a year old, to answer your question drseltsam, I've personally never heard of using both in the same wash without filtration, but I would assume the purpose is to speed up the process, and not wait for the IPA to evaporate, and lose less product since there's no filtration.
 
I am not sure if we are talking about the same here. When you recrystallize a substance you can solve it in a solvent A and then add B to push the substance out of A again. A simpler form is to just use B in the first place.

I have done both methods but not for MDMA and I was wondering why poopstation was recommending this method.
 
With just using acetone to wash the MDMA, you will not get crystals. Because MDMA does not dissolve to acetone. Crystals form when a substance is dissolved inliquid and then forced out of that solution. That is to say: MDMA dissolves to IPA. You can force MDMA out of IPA for example by using acetone or to just letting the IPA to evaporate.
Though letting the IPA to evaporate does not give you the benefit of getting rid of cuts that would otherwise dissolve to acetone.
 
bla-ljus, thanks for your answer. I am well aware of the difference between an acetone wash and recrystallization, in fact I hold a degree in Chemistry. My question was if there is any advantage in using IPA to solve MDMA and then acetone to push it out again vs. just recrystallize from acetone (which is not an acetone wash). Any comments here?
 
You are more qualified than I am, I have no degree in chemistry. Just been reading lots of stuff, though one needs to remember to take everything that's in the net with grain of salt. There was nice forum on silkroad where one person was very skilled and informative. How do I know he was skilled? Well, not that many unskilled persons have videos about how to make cocaine and all the things he had. I did believe it was true as he said that he had been working for a drug cartell as chemist.

Anyway, back to the point: How do you "recrystallize from acetone"? MDMA does not dissolve into acetone. Well, it does _very_ slightly, can't recall the word used (immiscible?). I assume one would need a lot of acetone and patience to recrystallize with acetone.
 
You are right at room temperature. You have grind the mdma to a fine powder and then dissolve it in boiling acetone. Ideally under reflux. From what I have found, you should need about 50ml per gram. This makes it very attractive for handling 1-3 grams as you have to handle around 150 ml. When using IPA/acetone you would need to handle 10 ml of IPA and 40 ml of acetone.

I would suspect that the crystallization works slower but from a higher concentration when using IPA/acetone. This should give you more medium size crystals, which is what you want. Big crystals often contain a lot of solvent which you have to get rid of before you consume the mdma

I would not advice to try any of this without extended experience in a chemical lab. The risk of consuming the acetone if you do it wrong is too high.

I highly doubt that an acetone wash is wort the effort. You wil only clean the surface of the crystal and make it look good.
 
For acetone wash, I put the acetone to freezer (-18c), use about 10cl of acetone (I have a shot glass I use) for 1-2gr of MDMA. The MDMA is crushed to powder and having it in the acetone seems to make powderizing it even easier. The result usually is brown tint to acetone, while the brownish powder will turn to snow white. My process is not perfect and there is some substance loss, but I rather have MDMA powder which is likely to be free of most cuts. Makes it easy to get consistent dosing across the different batches.
 
Great that this works for you!

Two comments:

You can try to reduce your losses when you dry the acetone with the help of epsom salt. Just make sure that you remove the water from the epsom salt by heating it up in the oven before usage. Google is your friend and there are plenty of good instructions around that you can find with good.

An other way could be to dry the MDMA first by putting it in a air-tight container with fresh silica gel to remove the water from the MDMA itself.

I respectfully have to disagree with you that this procedure will remove cuts from MDMA. If your MDMA is cut with lactose, PMA/PMMA or similar. This will not be removed. You will mainly remove the precursors from the synthesis like Safrol which causes the smell some people think good quality MDMA has but in fact is tells you that the chemists who made it did not clean the product properly. Thus, if your MDMA was cut deliberately you have no change of getting rid of it.
 
The procedure described by poopstation works well. I think 3 ml per g is a bit too much but you should it add it gradually anyway. I did not see why one wants to add freezer chilled acetone to the IPA. If the IPA is at room temperature, I just used room temperature acetone to ensure slow crystallisation. Recovered 80% of the initial mass.
 
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