Racemic MDMA, single-crystal structure

[scureto1]

It seems to be conventional wisdom among a lot of posters that I've seen here on BL that MDMA.HCl can not form large crystals because of the two enantiomers present. However, this paper seems to suggest that a single crystal can contain both enantiomers.

http://library-resources.cqu.edu.au/JFS/PDF/vol_44/iss_4/JFS4440761.pdf

The authors did some crystal structure and conformational analysis on single-crystal samples and came up with a crystal structure that they say was subsequently confirmed by another group's findings. The structure they determined does include both enantiomers (the figure only shows one, but in the corresponding text they state that it includes both enantiomers.

I have personally seen some variations in crystal size based on recrystallization techniques, so I had been doubtful of the "no large crystals" argument, but this seems to finish it off.

Any thoughts?

 

[pofacedhoe]

do people honestly believe that when you buy crystal mdma that its one isomer? really?

 

[scureto1]

I haven't seen many, but there is persistent speculation among a few that some of the Dutch superlabs might be doing some enanantiomeric separation. I try my best to point out why that just isn't reasonable, but it always seems to pop back up.

I think the whole debate pops up because of the constant talk about "moonrocks", which, to me, just look like someone is heating up MDMA.HCl crystals to a point where they become amorphous and then mashing them together so that they LOOK like a big crystal to people who don't really know what a "single crystal" means. Then, others will respond with something along the lines of: "If it is one big crystal, then it is definitely either not MDMA or it is adulterated MDMA, because MDMA is racemic and can't form large crystals."

I don't think "moonrocks" are actually single crystals or anything like that, but based on the findings in this paper, it is clear that racemic MDMA can form large crystals.

 

[futura2012]

I dont know if your saw my post on ED scure but this was a recent isomer resolution guide I found.

To my untrained eye it looks relatively simple but I might be wrong?

I will try and dig out some info for you about the crystals also.

MDMA isomer extraction

2,00 g (10mmol, assuming 95% purity in the Islands) distilled MDMA
0.75 g (5mmol) D-tartaric acid
3ml H2O
6ml xylene (which turned out to be handy)
A solution of NaOH, equivalent to 0.2 g (5mmol) NaOH.
! Not use solid NaOH! Only solution! Hard has a different concentration of active ingredient and water, that a very strong impact on the results of separation: if the D-isomer is allocated fairly well, but a net L-isomer is unlikely to succeed. The easiest way to prepare the solution - dissolve a handful of alkali in the glass Dist. water, cooled to room temperature, weighed in a volumetric flask, calculate the density and concentration. Well or titrirovat - who like more.
And then weigh the required amount of solution.

After mixing the reagents, a lot of shake up and leave for a day. Xylene solution of L-MDMA separate, additional water rinse xylene. To add the excess xylene halophytes and leave to evaporate, first in the air to the evaporation of xylene, and then in a desiccator over NaOH. Obtain 1,05 g caramels. Rub the several times with acetone, ignoring the losses and obtain 0,6 g R (-) MDMA (L-MDMA).
An aqueous solution of D-MDMA alkalizes twice ekstragiruem, add soup and dried. Obtain 1,1 g of crystalline S (+) MDMA (D-MDMA).

 

[scureto1]

Yes, you posted that in ED and I've discussed it with you there. "Not reasonable" isn't the same thing as "not possible" or even "not easy". I've gone into why at length in the other thread. This one is about racemic MDMA forming large crystals.

edit: Just realized that my link to the journal article was broken. Fixed now.

 

[futura2012]

I have been reading some other sites and this seems to be one method to get big Xtals from Racemic MDMA.

Looks impractical but certainly makes the theory possible

Takes forever though. They usually don't do this unless they're crystallizing proteins or some ridiculously hard to crystallize structure. Awesome crystals though

? Solvent added (clear) to compound (orange) in first vessel to give compound solution (orange) ? First vessel is placed in a second vessel contain second solvent (blue). The second vessel is sealed, the first vessel is also sealed, although a small hole in the first vessel is present. This hole allows volatile solvent vapour (blue) to slowly evaporate from second vessel and condensate (that is infuse) into the first vessel, to give a mixed solvent system (green) ? Over time this gives crystals (orange) and a saturated mixed solvent system (green-blue).


This link is relevant to your discussion topic also:

http://www.ualberta.ca/~csps/JPPS1(1)/A.Mitchell/racemicview.htm


Some bee posts to illustrate where the concept comes from

If its a racemic mixture (which is more than likely for MDMA) you wont get shit regardless of the method mentioned above. You need to separate the enantiomers first.

Its true that you will obtain small rhombohedral crystals with racemic MDMA, but not large shards like the OP is asking. For getting the latter you need to separate the enantiomers.
Crystallization has nothing to do with polymerization.

Anyways, can't the isomers be separated using tartaric acid, assuming it is isometrically pure? If the isomers were isolated, they would then be able to form large crystals of both the isomers. They would likely have noticeably different effects, wouldn't they?

appearance means little. there any many different techniques and solvents you can use to crystallize mdma in, each giving different looking salts. just focus on getting it as pure as possible by whatever means are available to you, don't put all your money on appearance. if you have shards of mdma then its adulterated

Did I ever said that all racemic mixtures didnt crystallized ? Stop being a theoretical chemist and get in the lab youll see that it is not possible to crystallize large crystals of RACEMIC MDMA.

racemate MDMA may not form large crystals, but 'shards' or 'rocks' can be made by fusing the hydrochloride (this is how the canadians and dutch produce 'crystal' mdma)

first off, as stated correctly, racemic compounds will not form shards. if you have ever seen MA made from P2P (that has not been resolved via tartric acid), you do not have shards at all. you have 'powder'...

 

[sekio]

This thread is kind of fluff filled, it may be better off in ED
It is totally possible to grow xtals of racemic MDMA but of course it will be mre difficult than crystallizing a single enantiomer.

 

[futura2012]

I think this topic is well out of the range of ED Sekio.

I understand fragments of it but nothing like the detailed discussion I think scure is hopefully looking for.

I have just thrown some snippets in there to hopefully help along.

If you can keep it rolling here would be very interested to see some of the ADD responses.

Hope you dont mind.

 

[sekio]

MDMA.HCl can not form large crystals because of the two enantiomers present.

Where did this thought come from? Racemic compounds can form crystals just as well as single enantiomers. Both enantiomers will crystallize at the same time - sometimes they will co-crystallize.

It looks like the xtal structure published in the first post is not a racemate, it's a single enantiomer.

 

[scureto1]

From the end of the 1st paragraph on pg. 765:

"Both enantiomers are present in the crystal but the structure in Fig. 1
shows only the S-enantiomer. This figure is drawn to show the hydrogen bonding clearly."

I indicated that in my OP.

As for where that thought came from, I have no idea. That's what I meant by conventional wisdom - one of those things that "everyone" seems to "know" but for which they have no evidence.

There are cases where racemates can't be part of the same repeating crystal structure - if one of the groups coming off of the stereocenter has some steric bulk, each enantiomer has to take a different conformation in order to keep that bulky group out of the crystal face. With different conformations and thus different 3-dimensional shapes, the two enantiomers can't make a repeating pattern, so "mismatches" effectively end individual crystals, making it impossible to grow large, regular crystals.

It looks like perhaps that isn't the case with MDMA, however. I suspect it is because the relevant group on the stereocenter is just a methyl, so neither enantiomer has any steric issues.

 

[amanitadine]

What the fuck is this garbage? Half the shit above is barely intelligible.. .

I never had an issue with creating large crystals of racemic MDMA. Sure, they weren't "shards" like d- meth, or whatever the hell the kids are calling it nowadays, but 500 mg rhomboids were possible with a very slow recrystallization in IPA, from boil to RT to fridge to freezer over 24 hours.

And yes, all the "moon rock" garbage is exactly that (garbage, not moon rocks), and has been melted and smashed up. But that's what sells! Meh.

 

[scureto1]

The shit above is textbook chemistry. It is used to explain and often predict your cookbook chemistry.

 

[amanitadine]

Ha ha Good answer! By " above" I meant the thread, in particular the dude with the bee, and as it applies to MDMA, your post is solid.

 

[futura2012]

What the fuck is this garbage? Half the shit above is barely intelligible.. .

Ha ha Good answer! By " above" I meant the thread, in particular the dude with the bee, and as it applies to MDMA, your post is solid.

All the information there is from another synth forum I am a member of. It is from a thread where the OP has requested known methods to make large crystals of MDMA.

All the quotes are from other members they are not my own words.

The only thing I will add is a lot of those quotes are likely from people actually cooking MDMA in some way. Obviousley I cannot guarantee that but it would seem that way.

The theory of racemic MDMA not producing large crystals doesnt just come from one person but many people seem to think the same thing. I have heard this from a variety of sources.

I put that information there to assist with the discussion if you feel it is of no use I would be more than happy to edit it out.

Could you be more specific which piece of information or quote you think is garbage?

I never had an issue with creating large crystals of racemic MDMA. Sure, they weren't "shards" like d- meth, or whatever the hell the kids are calling it nowadays, but 500 mg rhomboids were possible with a very slow recrystallization in IPA, from boil to RT to fridge to freezer over 24 hours.

500mG rhomboid sounds very interesting. Would be very interested to see what that actually looks like. Would you be happy to show a pic?

All the moonrock stuff that people upoad on ED is fused. I have never seen anything like what you describe. Particularly if you can complete the process in 24 hours with such a simple method.

Below are some pics of Racemic Structures which are rhomboid but much much smaller. Also a fused "Moon Rock" to show a comparison:

MDMA Racemic Crystal Formation 1

MDMA Racemic Crystal Formation 2

MDMA Fused "Moon Rocks"