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What is wrong with the MDMA available today? - v2

I did point out that MDMA hydrochloride can be melted without any solvent being present and as it cools, it will return to it's solid state.

So yes, absolutely heat is almost certainly one of the key tools. I'm not entirely certain how you would consider using pressure. To press microcrystals into a block?

I found a few more images of 'moonrock' and understand (I think) why that name was chosen. The first images I found didn't make it clear.


There is no clear crystal lattice but there are voids (holes) and that second moonrock from the left has a flat surface. As if it's solidified against a surface.

So I would guess that a (possibly pyrex) vessel was filled with microcrystalline MDMA hydrochloride, the vessel was heated until all of the product melts and then it was allowed to cool. As you can imagine, even if you press down on a powder, there will still be tiny air pockets. It's my suspicion that the voids are the result of that air flowing together and forming bubbles.

So I guess that when MDMA hydrochloride melts, it's still a thick (high viscocity) liquid. Maybe something like clarified honey. Maybe a little thicker. That being the case, those voids won't bubble up very quickly hence those sperical holes in the moonrock.

It MAY also explain the colours. It may be the case that if the melting and setting process aren't carried out under dry nitrogen (or other cover gas), it's possible that the MDMA oxidizes or otherwise changes chemically.
The one thing I now understand (I think) is that by performing the melting and casting of the product, it will be at or near it's maximum density. If a given weight takes up less space, it's easier to smuggle. As you mentioned, it's also possible that intermediates were left in the product and at least some of them will form dimers. So while the product may not become 'less pure', it could be the case that the impurities change.

I also note that the second rock from the left seems to be composed of two different coloured layers. I don't know why that should be the case but one theory is that a liquid layer of product was poured onto a previously cooled layer of solid product. It looks like the voids are more common in the lighter coloured layer i.e. the air bubble were rising.

But one thing is for sure, there is no reason why moonrock is inherently purer than the microcrystals that were around 30+ years ago. BUT it does mean that a cutting agent could only be added before the product was converted into moonrock. No middleman could bulk it out. So I think I can see why people might trust it more.

I guess we all like our own product and for me, those sparkly white microcrystals are what I am used to. One thing that EVERY reference agrees on is that when pure, the product is a brilliant white. But then, so are many cuts. So while a brilliant white doesn't prove purity, any other colour proves lack of purity.
Here's a photo "fake/forced" moonrocks

 
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Here's what it "Should"


suppose to look like "Proper" moonrocks that is racemic,






Hope that helps @4DQSAR

Sadly what I remember of "how it was done", I didn't understand crystallography, let alone my synthesis knowledge was lacking back then...

It's just what I remember from a "Dutch" forum probably back in 2012-14/15 not later then 2018 for sure... but kinda lines up... So if i'm wrong... well I don't know shit for chemistry XD
 
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I've just remembered something. Years and years ago someone gave me a load of chlorocaine hydrochloride - the one that came before 'nitrocaine'. Before you say it - yes, they WERE both rubbish. But they were both white, sparkly powders.

But the reason I mention it is that I was asked if I could make 'big crystals' and I just put some of the powder into a Pyrex dish and put the dish in the oven. I know, dumb. But the stuff was more or less waste anyway and it cost me nothing. Anyway, when it melted, it was REALLY thick. I mean like clarified honey or maybe melted sugar. THICK and gloopy. As it got hotter, it got less and less gloopy.

When I took it out of the oven it had turned yellow. Not a deep yellow but definitely not white. It didn't freeze as I expected it to do. What it did was slowly get thicker and thicker until it was something like beeswax, You could push a sharp knife into it but I couldn't mark it with my fingernail (for example).

Now the two chemicals are totaly unrelated. The only thing they share is that they were hydrochloride salts. Oh, and there were voids (bubbles) in it.

So I'm beginning to wonder if, when I melted it, what I ACTUALLY got back was an 'amorphous' form of the stuff. It didn't suddenly go from a liquid to a solid, it just got thicker and thicker. What is the texture of the stuff you have like? Is it a crystal you can shatter? Does it crush up into a fine powder?

Needless to say, I jus threw it away my ailed experiment and forgot about it,

But whatever the details, I'm pretty sure moonrock is made to stop mid-level dealers from cutting the stuff and almost certainly going to get the most product into the smallest space.

Moonrock - it's a strange idea but the more I think about it, the more sense it makes.

Oh- I would also guess it would smell less. Does it have an odour?
 
I've just remembered something. Years and years ago someone gave me a load of chlorocaine hydrochloride - the one that came before 'nitrocaine'. Before you say it - yes, they WERE both rubbish. But they were both white, sparkly powders.

But the reason I mention it is that I was asked if I could make 'big crystals' and I just put some of the powder into a Pyrex dish and put the dish in the oven. I know, dumb. But the stuff was more or less waste anyway and it cost me nothing. Anyway, when it melted, it was REALLY thick. I mean like clarified honey or maybe melted sugar. THICK and gloopy. As it got hotter, it got less and less gloopy.

When I took it out of the oven it had turned yellow. Not a deep yellow but definitely not white. It didn't freeze as I expected it to do. What it did was slowly get thicker and thicker until it was something like beeswax, You could push a sharp knife into it but I couldn't mark it with my fingernail (for example).

Now the two chemicals are totaly unrelated. The only thing they share is that they were hydrochloride salts. Oh, and there were voids (bubbles) in it.

So I'm beginning to wonder if, when I melted it, what I ACTUALLY got back was an 'amorphous' form of the stuff. It didn't suddenly go from a liquid to a solid, it just got thicker and thicker. What is the texture of the stuff you have like? Is it a crystal you can shatter? Does it crush up into a fine powder?

Needless to say, I jus threw it away my ailed experiment and forgot about it,

But whatever the details, I'm pretty sure moonrock is made to stop mid-level dealers from cutting the stuff and almost certainly going to get the most product into the smallest space.

Moonrock - it's a strange idea but the more I think about it, the more sense it makes.

Oh- I would also guess it would smell less. Does it have an odour?
Sometimes, It smells like anise, safrole or MDP2P glycatesish.... sometimes, it smells like "chrome"/metal when I've had Purple and especially Green MDMA
 
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. Years and years ago someone gave me a load of chlorocaine hydrochloride

Sold as: MDMA
Expected to be: Not Specified
Note
SaferParty issued an information alert because this powder contains a drug other than MDMA and could be mistaken for MDMA.

Per the testing organization's alert, the sample probably consists of 'a resin product resembling MDMA crystals that has been treated with chloroquine (a malaria medicine), which has a bitter taste'.

I would imagine they would find it.

But maybe if the lab isn't looking for it. They won't see it.
 
So

A year or 2 back I recrystallized some white MDMA. Almost snow. But removed some purple crap.

Eventually

Got 2 different trapezoids

1 clear long shard that looked great VERY see thru almost like glass. But was brittle/weak. I live in a high humidity area. Probably was the last crop after months and months. And was dud meh horrible no effect, I don't remember if I lab tested it but I assume I did. Gave some to multiple people. They all said it was meh...

The second though I haven't tried

But if I find it it matches the "proper moonrocks" as described. I'll see if I still have examples of both.

Is it a crystal you can shatter? Yes

Does it crush up into a fine powder? Yes but I use a motor a pedestal
 
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Thanks for providing that information.

Those voids (bubbles) that were in some of the images. I presume that is why people call it 'moonrock' so is it usual to see such things?

One thing I know is that if a compound is impure, it won't have a sharp melting point. It will tend to soften before actually melting.

I'm sure it's possible to figure out how it's made and I said why I think it's being made that way, but you mentioned it containing impurities so moonrock isn't absolute proof of purity, if I understand you correctly.
 
Thanks for providing that information.

Those voids (bubbles) that were in some of the images. I presume that is why people call it 'moonrock' so is it usual to see such things?

One thing I know is that if a compound is impure, it won't have a sharp melting point. It will tend to soften before actually melting.

I'm sure it's possible to figure out how it's made and I said why I think it's being made that way, but you mentioned it containing impurities so moonrock isn't absolute proof of purity, if I understand you correctly.
Never seen bubbles in my moonrocks.

I've seen it as more "fuzzy" almost like microcrystalline structure protruding

And not crisp defined crystals. Like how it should be.
 
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I found a few images of very large moonrocks and there were definitely bubbles in it.

Maybe moonrock is just a blanket term for the product of one particular synthetic route? Quite often the names are made up by distributors, the chemists normally just use the word 'product', whatever they happen to make,

I'm glad you pointed it out.

The last I heard PMK glycidate was the most common MDMA precursor. People converted PMK glycidate to PMK and then used one of the known routes to make MDMA from PMK. I know the 'holy grail' was a direct route from PMK glycidate to MDMA. Who knows? Maybe someone found a way and moonrocks are how the product ends up.

After all, if the result is good and the price goes down, consumers will happily accept a new form of the stuff.
 
I found a few images of very large moonrocks and there were definitely bubbles in it.

Maybe moonrock is just a blanket term for the product of one particular synthetic route? Quite often the names are made up by distributors, the chemists normally just use the word 'product', whatever they happen to make,

I'm glad you pointed it out.

The last I heard PMK glycidate was the most common MDMA precursor. People converted PMK glycidate to PMK and then used one of the known routes to make MDMA from PMK. I know the 'holy grail' was a direct route from PMK glycidate to MDMA. Who knows? Maybe someone found a way and moonrocks are how the product ends up.

After all, if the result is good and the price goes down, consumers will happily accept a new form of the stuff.
Pretty sure helional to mdp2p or otherwise is starting to become the norm... but who knows.

I've thought about starting from piperonyl acetate to piperonal as well.

I'm also sure some are even using catechol as 1,2 methylenedioxybenzene

Then to 3,4-methylenedioxymandelic acid by reacting 1,2-methylenedioxybenzene...


Then convert piperonal using the Wittig reaction

Or



Synthesis of 3,4-(methylenedioxy)-beta-nitrostyrene by Henry condensation of piperonal and nitromethane. You would get it Hydrocinnamic alcohol derivatives I think? Then go to a nitriles or oxime.


I know know moon rocks as LARGE chunks of MDMA.

Multiple different colors. Assumed different routes.
 
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Impressive that you know so many diverse routes to MDMA.

I noted on multiple HR sites that 'purple moonrock' was prevalent last year. Someone used MCMC analysis (or something equally sensitive - I forget exactly what methadology was used but it's commonly able to identidy chemicals in the parts-per-billion range) and they couldn't find a known dying agent or indeed any consistant impurity that was being added to produce that colour.

It wasn't pure, there were traces of other chemicals but sadly I couldn't find a list. But my point is nobody was adding something to make it purple. Given that MDMA has a very basic amine moiety, I would suggest that either the impurities themselves contain a basic amine so A/B extraction won't remove them OR the makers don't use an A/B extraction which would save a lot of time and a lot of solvent. So it makes financial sense to omit the step if possible. That would then mean safrole, piperonal or whatever to end up in the product.

But it did make me think about crystals. We identified the crystal structure of pure MDMA which showed that the raecemate COULD produce crystals but Nichols et al were in the position of having access to extremely pure samples.

But it's well known that many crystals take on a colour if they are impure. Even diamonds can have colours. In fact, they can be almost any colour, even black. In fact the black diamonds are used industrially as they are the hardest type of diamond. In that case the intercallanation of different allotropes of carbon is what increases the hardness, So any test would show that only carbon was present i.e. no chemical impurity.

So if someone has an extremely large crystal of almost any impure crystalline solid, those intercallantions will possess different bond-lengths and it's more likely than not that some of them will absorb certain frequencies of visible light.

So I think you are quite right in saying that the colours are likely to be artifacts of the impurities. They interrupt the crystal lattice and assuming that the impurities are equally spaced throughout the lattice, it will result in a specific colour.

It would be possible for someone to purposefully add small quantities of various known impurities and go on to produce crystals so the colour might identify the specific impurities.

So I got there in the end!
 
BTW pieronal, PMK, safrole and even sassafras oil are explicitly controlled under Chinese law. I'm well aware that there are dodgy suppliers who will happily BREAK the law but the fact that the glycidate easter/salts were being offered in large quantities from a lot of Chinese sources suggests that they were operating in the gray market. They pretend not to know what the product is used for and under local law, they aren't doing anything wrong. But it did seem quite costly.

Also the glycidate esters/salts are commonly made from piperonal or PMK.

It's that methylenedioxy ring that makes it tricky. Yes, you can build that bridge but again, it's costly.

One thing I know about the Chinese is that they always look for the cheapest way to do something. So I took a look at other natural compounds with that bridge. One sprung out at me. It's found in the essential oil of a food crop commonly grown in China. It can be cleaved into piperonal in very high yields (96%). There is another source. The essential oil of a herb undergoes basic hydroxlysis to yield exactly the same, legal intermediate.

So I can see that if the natural product is much cheaper than the glycidate esters/salts that were previously offered, it would make perfect sense.

You said piperonal, these would yield piperonal via a simple oxidative cleavage.

On the surface piperonal takes more steps to produce MDMA but there are people who specialize in telescoping down the complexity of a syntheis.
 
BTW pieronal, PMK, safrole and even sassafras oil are explicitly controlled under Chinese law. I'm well aware that there are dodgy suppliers who will happily BREAK the law but the fact that the glycidate easter/salts were being offered in large quantities from a lot of Chinese sources suggests that they were operating in the gray market. They pretend not to know what the product is used for and under local law, they aren't doing anything wrong. But it did seem quite costly.

Also the glycidate esters/salts are commonly made from piperonal or PMK.

It's that methylenedioxy ring that makes it tricky. Yes, you can build that bridge but again, it's costly.

One thing I know about the Chinese is that they always look for the cheapest way to do something. So I took a look at other natural compounds with that bridge. One sprung out at me. It's found in the essential oil of a food crop commonly grown in China. It can be cleaved into piperonal in very high yields (96%). There is another source. The essential oil of a herb undergoes basic hydroxlysis to yield exactly the same, legal intermediate.

So I can see that if the natural product is much cheaper than the glycidate esters/salts that were previously offered, it would make perfect sense.

You said piperonal, these would yield piperonal via a simple oxidative cleavage.

On the surface piperonal takes more steps to produce MDMA but there are people who specialize in telescoping down the complexity of a syntheis.
That's not even half of them they recently have switched from glycidate due to the ban, but they still ship it I heard, to

MDPADA, etc. The MDP2P twins of α-phenylacetoacetonitrile (APAAN), α-phenylacetoamide (APAA) and methyl α-acetylphenylacetate (MAPA)

MDPAA is also making rounds so I'm told.. more watched as it is MD phenylacetic acid..

Honestly I have a few my self, I don't want spoiled... All these have been spoken and talked about including,

Making MDA from Helional via the typical, Oxime, Hoffman, nitrile, etc, then converting to N-formyl-3,4-methylenedioxyamphetamine with 90-95% yield...

 
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One sprung out at me. It's found in the essential oil of a food crop commonly grown in China. It can be cleaved into piperonal in very high yields (96%).
So what MD compound is found in that essential oil ? Can you draw it ?
 
BTW pieronal, PMK, safrole and even sassafras oil are explicitly controlled under Chinese law. I'm well aware that there are dodgy suppliers who will happily BREAK the law but the fact that the glycidate easter/salts were being offered in large quantities from a lot of Chinese sources suggests that they were operating in the gray market. They pretend not to know what the product is used for and under local law, they aren't doing anything wrong. But it did seem quite costly.

Also the glycidate esters/salts are commonly made from piperonal or PMK.

It's that methylenedioxy ring that makes it tricky. Yes, you can build that bridge but again, it's costly.

One thing I know about the Chinese is that they always look for the cheapest way to do something. So I took a look at other natural compounds with that bridge. One sprung out at me. It's found in the essential oil of a food crop commonly grown in China. It can be cleaved into piperonal in very high yields (96%). There is another source. The essential oil of a herb undergoes basic hydroxlysis to yield exactly the same, legal intermediate.

So I can see that if the natural product is much cheaper than the glycidate esters/salts that were previously offered, it would make perfect sense.

You said piperonal, these would yield piperonal via a simple oxidative cleavage.

On the surface piperonal takes more steps to produce MDMA but there are people who specialize in telescoping down the complexity of a syntheis.
But my point is nobody was adding something to make it purple

When the purple hype started, my friend DID show me dyed product as it looked off? dude later admited to source he did indeed dye it. Was like 1 Kilo he got also :(

But it did look different then other purple stuff I saw
 
So I would guess that a (possibly pyrex) vessel was filled with microcrystalline MDMA hydrochloride, the vessel was heated until all of the product melts and then it was allowed to cool.
Yes, if this were the case, the vessel would be sodium borosilicate glass, but steel could technically work, too, at the sacrifice of visibility. At standard atmospheric pressure, MDMA.HCl will scorch and polymerize before it reaches its boiling point range. If put under a vacuum, it's possible this could be avoided, but I doubt most manufacturers would bother with this, which is difficult to do at volume. And I don't think it's necessary for producing so-called "moon rocks" anyway. But I also can't totally rule it out, either, so maybe?

So I guess that when MDMA hydrochloride melts, it's still a thick (high viscocity) liquid.
Not in my experience. It turns black and nasty as it burns, pyrolizes, scorches and emulsifies. Co-(re)crystallization from a two-solvent system seems more likely.

Maybe something like clarified honey. Maybe a little thicker. That being the case, those voids won't bubble up very quickly hence those sperical holes in the moonrock.
The freebase oil is more like yellow-ish clear clarified honey. I would guess the "voids" in the crystal structure are more likely the result of mixing patterns of co-crystallizing agents.

But one thing is for sure, there is no reason why moonrock is inherently purer than the microcrystals that were around 30+ years ago.
Agreed.

BUT it does mean that a cutting agent could only be added before the product was converted into moonrock. No middleman could bulk it out.
Similar to cocaine re-rock, MDMA could be re-rocked by some enterprising shitbag middleman, though to your point: it does seem less likely.

So I think I can see why people might trust it more.
I wonder how many people are thinking this hard about it. Either way, while this logic is flawed, I agree it's probably what many, if not most, people reason.

I guess we all like our own product and for me, those sparkly white microcrystals are what I am used to. One thing that EVERY reference agrees on is that when pure, the product is a brilliant white.
Bingo. I point this out all the time. The Merck Manual lists it as a bright white crystalline salt, and this is consistent with the MDMA.HCl I produced ~25 years ago. I also vacuum distilled both my ketone (made from sassafras oil/safrole) and my final product. I imagine discoloration is typically the result of an impure matrix, though food dye is also possible sometimes.

But then, so are many cuts. So while a brilliant white doesn't prove purity, any other colour proves lack of purity.
Right, an added diluent would likely be bright white, but reaction impurities that aren't removed are more likely to produce colors like tan, beige, champaign, purple and/or pink. Scary ain't it? Yet the majority of discolored MDMA I've had was 🔥 too, so I don't think any of this is sufficient to prove that the cause of some people's "mehDMA" experience is solely the result of suboptimal production techniques…
 
So what MD compound is found in that essential oil ? Can you draw it ?


Voila.

Interesting that people were so keen to argue the toss without even appearing to understan the chemistry.

It seems that @vash445 has much more intimate knowledge of what is actually going on in current MDMA production that anyone else I've talked to, so I've checked and everything they say FITs. Put simply, people make MDMA for MONEY. If they can find a cheaper route, they will ALWAYS use that cheaper route. Grisham's law demonstrates that such will always be true. You can always sell your product for less than someone with higher costs.

A few years ago the glyciadate esters/dalts of PMK were being sold by Chinese suppliers BUT it was quite costly.


Here are a couple of the possible esters but the truth is, there are in theory HUNDREDS of facile esters. One could just as easily supply the lithium, sodium or potassium salts BUT because they are a much smaller group of compounds, it would be simple to ban MD glyciades and it's addition salts.

There are other, less well known essential oils that will yield piperonall in very high yields (>96%). So as long as you design your synthesis in a manner than means that the major impurities can be removed simply and cheaply (vacuum distillation), that makes sense as the logical way to being down costs. Reacxt it withnitroethane (legal in Russia) yields the nitroalcohol or the nitroalkene. But in either case, it's simple to produce PMK from either.

I did identify the crystal structure of MDMA as confirmed by Nichols et al. I then went on to explain that even minor impurities in crystals commonly produce colouring. More formally, 'regular intercallination of crystalline structures commonly result in said crystals absorbing specific frequencies of visible light'.

I've seen 99.99% pure MDMA and it's a pure white crystaline solid. But I'm aware that both safrole and piperonal will result in samples that tent to be brown. But to be clear, those were always microcrystals. So it's possible that the impurity was on the surface of the crystal. But it's not that the presence of impurities of impurities resulting in coloured products is a new idea.

Black diamonda (carborundum) are uned industrually because they are harder than white diaonds. Why? Because there is an intercallanation of the regular crystal structure of doamonods with both carbon nonotbes and graphine (single molecular layers of carbon in a hexagonal structure), both of which are aromatic which increases the hardness,

Now I freely admit that this is all new to me, but I've had enough experience to know that when someone sets out to make an illegal drug, they don't seek to produce an impure product. At large scales, buyers DO test the product so you can't cut it and have them not notice the fact.

So it seems that moonrock is the result of someone who has worked out a way to produce very pure MDMA in a cheaper way. Believe me, people will pay a LOT for such information.

A friend of mine was paid 6000 euros just to write out a step-by-step synthesis of LSD analogues that relied on PyBIOP for the crucial step. Without PyBop the highest yield is around 65%. Using PyBOP the product is typically 95% pure. Pur enough to avoid the need for preparative chromatography. While PC isn't hard, it doesn't scale well - THAT was the really important thing. It avoided a bottleneck.

I haven't said which precursors I THINK may be involved, but the important thing is that both are cheap, both are legal and both are Commonly grown in China.

TBH at some point someone else will figure out that 7,a-DMT is 2-3 times more potent than MDMA and produces almost identical subjective effects. It's even legal in most placces. I expect even adjusted for cost-per-dose, moonrock is sill cheaper, but I predict 7,a-DMT WILL turn up in pills. 40mg is like a really strong pill ad since it;s legal, there will be some people who decide to openly order if - I mean, why not?
 
@vash445



It's worth reading the above paper. It explains that with only a single exception, all of the impurities previously found in MDMA hydrochloride are easily removed using an A/B (acid-base) extraction. The exception is a class. MDMA derivatives that have chlorinde and or bromine ions on the aromatic ring.

So they become part of the very MDMA molecule itself and would require an extremely costly and complex seperation technique to remove. Of course, it's hard to know what the subjective effects of 2-bromo MDMA, 5-bromo MDMA or 6-bromo MDMA are. Chlorine ions have also been detected:


So:

3 monosubstitutions
2 disubstitutions
1 trisubstitution

But double that because the -Br ions can just as easily be -Cl ions. Then consider the mixtures of disubstitutions (8) and trisubstitutions (8) and in fact, that's a LOT of different impurities.

I think that's a very important detail. It seems like MDMA producers are going from precursors to pre-precursors and now to pre-pre-precursors.

I've since looked at a lot of vendors quoting a purity of the product (monrock). I was originally confused because the pure white microcrystals that were common in the late 1980s and early 1990s were essentially 100% pure. Because producers performed the proper A/B (acid-base) extraction that would remove safrole, isosafrole, piperonal, PMK or any of the reagents that were carried through to the final workup. So now I see moonrock on offer with the purity stated as being anywhere from 92% to 96%. It's none of those intermediates I mentioned that are ending up in the products, it's the brominated or iodinated derivatives OF MDMA that are present.

That would also explain the differing colours. The C-Br and C-Cl bond-lengths differ and differ again depending where they are on the rings and what other ring-substitution is present.

I should add that if a laboratory is prepared to srart from benzodiozole, it's a LOT more work:

Benzodioxole + Bromine ---> 5-bromo-2H-benzodiaxole (which will also dibrominate to the 5,6-dibromo, tribrominate or even tetrabrominate). But all of those will then undergo.

1) 5-bromo-2H-bromodioxone (or homologues) + Magnesium metal ---> 2-methyloxirane ---> 1-(2H-1,3-benzodioxol-5-yl)propan-2-ol (or homologues)

2) 1-(2H-1,3-benzodioxol-5-yl)propan-2-ol + NBS (N-bromosuccinamide or TEMPO + Bromine or sodium hypochloride ---> PMK

There are two important things about rhe above. It's only practical at large scales and it involves the use of bromine in two routes and I GUESS that sodium hypobromite would also be possible and if you already have need for bromine gase (very toxic), simply adding bromine to sodium hydroxide solution would produce sodium hypobromite so it would reduce the price slightly. But ring-chlorination of samples has been seen, so clearly sodium hypochloride is used, at least sometimes.

Now right up to the point where PMK is produced, all of the above is legal. I also note that both piperonal and PMK can both be used to produce PMK glycidate. It's entirely possible fo the two synthetics stesps in which first piperonal or PMK are produced and the step to prodice the legal PMK-glycidate are carried out in a single reaction vessel. I'm not an expert in chemical enginerting but it may be that instead of a batch process, the syntheis uses a continuous flow process so even if the police were to visit the production line, they would only even find small quantities of controlled precursors as they are made and converted into a legal intermediate in the same system.

But given the syntheis explained by the paper, even if ONLY 3,-4-methylendioxy <ring halogenated> methylamphetamines are in the product, that's a possible total of 62 compounds.

Unlikely to be present in toxic amounts, but THAT is why we are seeing HUGE crystals. When being taught organic chemistry, it's repeated that ONLY pure(ish) samples will form crystals and the melting-point and melting-range of the crystal gives an insight into the purity. The higher the melting-point and the smaller the range over which the crystal melts is considered a spot-check for purity.

But if my other theory ic correct, manufacturers are producing MDMA hydrochlorideand the final step is the heating of the product to above it's melting-pount (either under a vacuum or using a protective atmosphere such as dry nitrogen) to remove ALL of the other types of impurity and then allowing the product to slowly solidify. If one is considering blocks weighing many kilograps, it will inhernetly be slow, but it's possible that the heating and cooling is carried out in an insulated vessel. After all, if all you have to to is to leave it to stand for 24 hours, is that a problem?

I would love to know just what scale these labs are working on. Whoever has managed to achieve a route that at once avoids the legal control of precursors, provides for large-scale prodution and a route that allows semi-skilled workers to carry out production.

But as you said - the colour surely WILL tell you exactly what impurities there are in a sample. It's possible to calculate the bond-lengths for every C-Cl and C-Br bond so it's possible to take the date used to produce figure 2 and to find use it to find how much of each impurity is present and therefore have a pretty good idea of which factory produced the sample.

That is one of the few advantages of following Shulgin's route and repeating the extraction process twice or even three times. If your product truly is 100% MDMA hydrochloride, it's chemically identically to eavery other sample of 100% pure MDMA hydrochloride. Yes, microcrystals, packaging and other forensic techniques can be applied, but the drug itself tells no takes.

Sorry to have gone on about if for so long. NOW I understand. Someone has found a route that makes the use of pre-pre-precursors a facile and dare I say it even a CHEAP route to make MDMA.

Amazing to think that in 1988 I used to pay £20 for a single 125mg MDMA tablet. But it was exactly that. What these people have been able to to is to reintroduce that potency but at a lower cost.

BTW I suppose the untimate would be for someone to produce (R) 7,α-DMT (7-methyl AMT). It's around four times the potency of MDMA and most people couldn't tell the difference between the two. For a while it was sold in Kokopelli as 'Empathy' but Dutch law changed.
 
@vash445



It's worth reading the above paper. It explains that with only a single exception, all of the impurities previously found in MDMA hydrochloride are easily removed using an A/B (acid-base) extraction. The exception is a class. MDMA derivatives that have chlorinde and or bromine ions on the aromatic ring.

So they become part of the very MDMA molecule itself and would require an extremely costly and complex seperation technique to remove. Of course, it's hard to know what the subjective effects of 2-bromo MDMA, 5-bromo MDMA or 6-bromo MDMA are. Chlorine ions have also been detected:


So:

3 monosubstitutions
2 disubstitutions
1 trisubstitution

But double that because the -Br ions can just as easily be -Cl ions. Then consider the mixtures of disubstitutions (8) and trisubstitutions (8) and in fact, that's a LOT of different impurities.

I think that's a very important detail. It seems like MDMA producers are going from precursors to pre-precursors and now to pre-pre-precursors.

I've since looked at a lot of vendors quoting a purity of the product (monrock). I was originally confused because the pure white microcrystals that were common in the late 1980s and early 1990s were essentially 100% pure. Because producers performed the proper A/B (acid-base) extraction that would remove safrole, isosafrole, piperonal, PMK or any of the reagents that were carried through to the final workup. So now I see moonrock on offer with the purity stated as being anywhere from 92% to 96%. It's none of those intermediates I mentioned that are ending up in the products, it's the brominated or iodinated derivatives OF MDMA that are present.

That would also explain the differing colours. The C-Br and C-Cl bond-lengths differ and differ again depending where they are on the rings and what other ring-substitution is present.

I should add that if a laboratory is prepared to srart from benzodiozole, it's a LOT more work:

Benzodioxole + Bromine ---> 5-bromo-2H-benzodiaxole (which will also dibrominate to the 5,6-dibromo, tribrominate or even tetrabrominate). But all of those will then undergo.

1) 5-bromo-2H-bromodioxone (or homologues) + Magnesium metal ---> 2-methyloxirane ---> 1-(2H-1,3-benzodioxol-5-yl)propan-2-ol (or homologues)

2) 1-(2H-1,3-benzodioxol-5-yl)propan-2-ol + NBS (N-bromosuccinamide or TEMPO + Bromine or sodium hypochloride ---> PMK

There are two important things about rhe above. It's only practical at large scales and it involves the use of bromine in two routes and I GUESS that sodium hypobromite would also be possible and if you already have need for bromine gase (very toxic), simply adding bromine to sodium hydroxide solution would produce sodium hypobromite so it would reduce the price slightly. But ring-chlorination of samples has been seen, so clearly sodium hypochloride is used, at least sometimes.

Now right up to the point where PMK is produced, all of the above is legal. I also note that both piperonal and PMK can both be used to produce PMK glycidate. It's entirely possible fo the two synthetics stesps in which first piperonal or PMK are produced and the step to prodice the legal PMK-glycidate are carried out in a single reaction vessel. I'm not an expert in chemical enginerting but it may be that instead of a batch process, the syntheis uses a continuous flow process so even if the police were to visit the production line, they would only even find small quantities of controlled precursors as they are made and converted into a legal intermediate in the same system.

But given the syntheis explained by the paper, even if ONLY 3,-4-methylendioxy <ring halogenated> methylamphetamines are in the product, that's a possible total of 62 compounds.

Unlikely to be present in toxic amounts, but THAT is why we are seeing HUGE crystals. When being taught organic chemistry, it's repeated that ONLY pure(ish) samples will form crystals and the melting-point and melting-range of the crystal gives an insight into the purity. The higher the melting-point and the smaller the range over which the crystal melts is considered a spot-check for purity.

But if my other theory ic correct, manufacturers are producing MDMA hydrochlorideand the final step is the heating of the product to above it's melting-pount (either under a vacuum or using a protective atmosphere such as dry nitrogen) to remove ALL of the other types of impurity and then allowing the product to slowly solidify. If one is considering blocks weighing many kilograps, it will inhernetly be slow, but it's possible that the heating and cooling is carried out in an insulated vessel. After all, if all you have to to is to leave it to stand for 24 hours, is that a problem?

I would love to know just what scale these labs are working on. Whoever has managed to achieve a route that at once avoids the legal control of precursors, provides for large-scale prodution and a route that allows semi-skilled workers to carry out production.

But as you said - the colour surely WILL tell you exactly what impurities there are in a sample. It's possible to calculate the bond-lengths for every C-Cl and C-Br bond so it's possible to take the date used to produce figure 2 and to find use it to find how much of each impurity is present and therefore have a pretty good idea of which factory produced the sample.

That is one of the few advantages of following Shulgin's route and repeating the extraction process twice or even three times. If your product truly is 100% MDMA hydrochloride, it's chemically identically to eavery other sample of 100% pure MDMA hydrochloride. Yes, microcrystals, packaging and other forensic techniques can be applied, but the drug itself tells no takes.

Sorry to have gone on about if for so long. NOW I understand. Someone has found a route that makes the use of pre-pre-precursors a facile and dare I say it even a CHEAP route to make MDMA.

Amazing to think that in 1988 I used to pay £20 for a single 125mg MDMA tablet. But it was exactly that. What these people have been able to to is to reintroduce that potency but at a lower cost.

BTW I suppose the untimate would be for someone to produce (R) 7,α-DMT (7-methyl AMT). It's around four times the potency of MDMA and most people couldn't tell the difference between the two. For a while it was sold in Kokopelli as 'Empathy' but Dutch law changed.
I was told .50 a gram on a new method
 
@vash445 I'm not quite with you. Do you mean the 'new method' only has 0.5% impurities?

I have noted that if you go back a while, 'purple moonrock' averaging anywhere from 92% to 96% was flooding the market. I hope I explained what the impurities were and why they would be next to impossible to remove.

I looked at a few sites that 'test' drug samples but they still seem to use presumptive testing. Well, aromatic halogens won't change the results of those. I decided to see if I could find some GC-MS (halogens would increase MW of material) and NMR (halogens replace hydrogens so people would be missing). I note 2-chloro and 2-bromo MDMA were the most common impurities but it seems like all the combinations I mentioned do or at least did occur:


I note more recent samples look a lot cleaner. I mentioned the possibility of swapping a batch-process for a continuous-process and one of the key reasons why the latter has become so much more popular is that as long as the product is being continuously monitored, it's possible to adjust the process in tiny steps to 'home in' on the best result.

The thing to remember is that even if 'only' 92% of the product is actually MDMA, that product is going to produce the same effects as MDMA. From a 'filling the role' perspective, it's fine.

The latesnt thing I noted was that the price of moonrock MDMA has now dropped below $1/dose (in bulk). I know, I know, nobody specifies how much a dose IS. If it's 100mg then $10000/Kg? If it's 125mg then it's a mighty $12500/Kg.

Now what I find interesting is that it's just another example of a model only working on a HUGE scale.

About a decade ago I met two Dutch guys who had figured out how to produce a 'bilayer' pill i.e. one face could be one colour, the other face another colour. The theory was that with nobody else having such technology they could exclusivley produce very high quality tablets each with 125mg in them. At that time in the Dutch market, producers were regularly making pills with 250-300mg in each and still charge a low price. I think they figured that ther would be a market for people who would pay extra to know exactly how much of exactly what drug was in each pill...

But if moonrock is SO cheap, nobody is going to pay ten times as much.

Grisham's law ALWAYS acts on the drug market.

What they really need is a new product. Such things exist, but nobody has figured a way to make them cheap.

Although the oxirane intermediate used in that paper would allow for 3,4-methylenedioxy 4MAR (MDMAR).
 
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