I don't but a lot of new work ups at least end of 2024 starting becoming more popular?
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MDMA &
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What is wrong with the MDMA available today? - v2
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4DQSAR
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Well I posted a link to a very fulsome article which gave the list of impurities, so we know several routes are in use.
The fact certain impurities were found suggests telescoping. The specific telescoping will depend on the specific route. But there are a lot of stratergies. Solvent-free reactions are one way to go. If one of the reagents is also a liquid with appropriate solvation properties, it also becomes the solvent. That is quite a common methodology. Not performing the usual B/A extraction saves a lot of solvent thus a lot of vessels and since it doesn't have to be removed, a lot of time. These are all things chemical engineers would know more about. Of course, a chemical engineer would generally perform a single purification step at the end of the process, not after each step.
As for 1-pot - if you have PMK, there is a 1-pot route that gives quantitative yields. It's not even a secret. BUT it does require a complex hydride reducing agent and I think we can all agree on is that whoever is doing the work has worked out what is an acceptable product and then has worked out the cheapest way of performing the synthesis.
I think what a medicinal chemist would think is that the goal is to produce a 100% pure product. What these people appear to have realized is that as long as the impurities are non-toxic, 94% purity is FINE. Of course, the other great thing about moonrock is that it would be a challange to cut. Goodness knows I've seen people take essentially pure MDMA and bash it with other powders to increase the profit margin. Pills used to be the way one prevented bad product. In the 80s it was the seal of quality. But then we found out that importers are buying presses and good pills, crushing and bashing the powdered pills and repressing the result.
At the end of the day, minimizing costs while ensuring maximum price is what the businessmen who now run such operations are after. There is no craftmanship. BUT there is profit. Much less than there used to be so scaling is the only way to go.
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unodelacosa
Bluelighter
Several newer routes might be in use now, but the lackluster experience phenomena predates this.
While your general observations about the economics and chemistry of illicit MDMA production are plausible, your statements sometimes oversimplify the complexities and challenges involved. Some chemical and logistical points need refinement. Claiming 'quantitative yields' from 1-pot PMK routes in clandestine labs is unrealistic due to limited equipment and control. While efficient 1-pot PMK routes exist, achieving truly "quantitative" (100%) yields in illicit lab settings is unlikely. These labs often lack precise equipment, controlled environments, and high-purity reagents. Yields are more likely to be high, but not perfectly quantitative.
Similarly, the assumption that ‘94% purity is fine’ overlooks the difficulty of assessing impurity toxicity and the potential for unpredictable effects. The assumption that these producers are capable of accurate toxicity assessments is questionable.
Furthermore, simplifying chemical processes like solvent-free reactions and final-stage purification ignores the challenges of illicit production. Inconsistent conditions and limited expertise often necessitate intermediate purifications and can hinder efficient, controlled reactions. While solvent-free reactions are a valid strategy, they can be more challenging to control – heat transfer and mixing can be less efficient, potentially leading to side reactions and lower yields. Plus, the risks of fires and explosions can increase. Finally, while cost is a driver, safety is often ignored, and 'cheapest' does not equal 'most efficient' in these uncontrolled environments.
ThreePointCircle
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I finally got round to sending my sample off to Kykeon. Sadly, they didn't find anything. Explicitly it seems they've excluded:
MDP2P Glycidate
MDDMA
MDEA
N-formyl-MDMA
Caffeine
6 1-(3,4-Methylenedioxy)phenyl-propan-2-ol
PMMA
MDP2P
PMA
3,4-Methylenedioxy benzyl-N-methylamine
Amphetamine
MDA
Methamphetamine
Here is the report
Was really hoping for an explanation for such a consistently bad experience but hopefully you will all find it useful data
MDP2P Glycidate
MDDMA
MDEA
N-formyl-MDMA
Caffeine
6 1-(3,4-Methylenedioxy)phenyl-propan-2-ol
PMMA
MDP2P
PMA
3,4-Methylenedioxy benzyl-N-methylamine
Amphetamine
MDA
Methamphetamine
Here is the report
Was really hoping for an explanation for such a consistently bad experience but hopefully you will all find it useful data
4DQSAR
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Well bromosafrole appears to be one intermediate that has turned up in samples. Now previously, it wasn't a popular route because amination is only efficient when the reaction vessel is under pressure (to allow heating to 130C). Also, it's an SN2 reaction so generally lower yielding.
But that assumed bromosafrole in methanol and 40% methylamine in water.
But think about it another way. If one has access to dry methylamine and pure bromosafrole, do you need a solvent? As long as the two are miscible, they are both the reagents AND the solvent.
I've noted a few patents in which copper catalysts allow RT amination which would avoid the need for a pressure vessel.
Now, obviously the products are MDMA and hydrogen bromide. Now secondary amines are more basic that promary amines so will the hydrogen bromide result in there being a single product, to whit MDMA hydrobromide. If that is the case, it's worth noting that such a product will NOT be soluble. That gives the possibility of a continuous process. bromosafrole and methylamine are added and slowly the reaction vessel fills with product.
Now that WOULD be the very cheapest route I know of. It's also worth noting that any of the three haloacids will add to safrole. So chlorosafrole would yield MDMA hydrochloride.
That's just one potential advantage of how telescoping can work.
-Solvent-Free
-Continuous process
-judicious use of catalyst to allow process to proceed at RT.
Back in the 80s and 90s, bromosafrole was known, but the need for a pressure vessel coupled by the use of solvents hugely increasing the volumes of liquids needed and finally, the need to employ pressure vessels meant it wasn't attractive. Somone who has just completed an undergraduate degree in chemical engineering would review all of the known syntheses to establish if they can be telescoped. A different mindset.
After all, it sounds like in Mexico, fentanyl is still 'cooked' from ANPP and propanoic anhydride* i.e. making precursors is a legally greay area but there are ALWAYS analogues that will keep it legal.
*Most people think of propanoic anhydride or at a pinch propanoyl chloride + scavanger amine are the only two reagents. This is not the case. In fact there are dozens - possibly even hundreds of related (but importantly UNCONTROLLLED) reagents that will work just as well. They are slightly more expensive, but can openly be ordered and delivered. When obstification is a key element of controlling production, SOMEONE will work out what is being hidden.
But that assumed bromosafrole in methanol and 40% methylamine in water.
But think about it another way. If one has access to dry methylamine and pure bromosafrole, do you need a solvent? As long as the two are miscible, they are both the reagents AND the solvent.
I've noted a few patents in which copper catalysts allow RT amination which would avoid the need for a pressure vessel.
Now, obviously the products are MDMA and hydrogen bromide. Now secondary amines are more basic that promary amines so will the hydrogen bromide result in there being a single product, to whit MDMA hydrobromide. If that is the case, it's worth noting that such a product will NOT be soluble. That gives the possibility of a continuous process. bromosafrole and methylamine are added and slowly the reaction vessel fills with product.
Now that WOULD be the very cheapest route I know of. It's also worth noting that any of the three haloacids will add to safrole. So chlorosafrole would yield MDMA hydrochloride.
That's just one potential advantage of how telescoping can work.
-Solvent-Free
-Continuous process
-judicious use of catalyst to allow process to proceed at RT.
Back in the 80s and 90s, bromosafrole was known, but the need for a pressure vessel coupled by the use of solvents hugely increasing the volumes of liquids needed and finally, the need to employ pressure vessels meant it wasn't attractive. Somone who has just completed an undergraduate degree in chemical engineering would review all of the known syntheses to establish if they can be telescoped. A different mindset.
After all, it sounds like in Mexico, fentanyl is still 'cooked' from ANPP and propanoic anhydride* i.e. making precursors is a legally greay area but there are ALWAYS analogues that will keep it legal.
*Most people think of propanoic anhydride or at a pinch propanoyl chloride + scavanger amine are the only two reagents. This is not the case. In fact there are dozens - possibly even hundreds of related (but importantly UNCONTROLLLED) reagents that will work just as well. They are slightly more expensive, but can openly be ordered and delivered. When obstification is a key element of controlling production, SOMEONE will work out what is being hidden.
unodelacosa
Bluelighter
Hell yes, in the 80s & 90s, talk of "pipe bomb" reactions + vessels were more common in clandestine lab forums – lengths of thick steel tubing w/a few Liters volume, threaded ends + caps welded shut once reagents + catalysts were loaded. It's muy Anarchist's Cookbook.
I heard stories of Bikers welding shut sealed 55-gallon steel drums for Al/Hg + CH₃NH₂ amalgam / reductive amination of p2p in aqueous solution under pressure. They'd tie a rope around the steel drum on one end, and tie the other to a tree near a river bank. Then as the reaction started, they would dip the whole barrel into the river for cooling. It would sizzle along and the reaction ran under pressure, and though probably not the most efficient conditions, there's still something badass and almost… elegant… about the sheer brutal simplicity of that reaction setup and its crude-yet-effective vessel. Selah.
Definitely not but so safe though. Hell, even in industry they renamed HPLC from "High Pressure…" to "High Performance Liquid Chromatography" because the word "pressure" tends to alarm insurance providers.
You make good points, though I'm still a bit dubious a clandestine lab would operate with such sophistication yet be the reason behind multiple batches of subpar product. If nothing else, the desire to stave off competition often adds some incentive for product optimization.
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4DQSAR
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HPLC - the L is for 'liquid'.
I'm pretty sure the name was changed because it's more accurate. You can have a vastly higher number of theoretical plates so it's possible to cleanly seperate componds with ALMOST idential MWs. A whole bevy of new types of chromatogrphy became possible as well.
Don't forget, the VOLUMES involved are tiny. Even if 1mL is at a HUGE pressure, it still doesn't contain much energy so doesn't represent much of a risk.
I am entirely guessing at what exact processes are involved, what I was trying to make clear was that there has been a huge paradigm shift. Even into the early 21st century there were people producing MDMA microcrystals and pilling them up on a vast scale. BUT moonrock entirely avoids the need to pill up the product - another saving. It's not a single improvement but freash eyes i.e. chemical engineers whose entire education is based on the idea that they will NEVER be dealing with a novel compound - that's medicinal chemist work. Chemical engineers look at how to scale a process and bing down costs.
A RT, solvent-free reaction that yields solid MDMA hydrochloride as the product would be an absolutely standard thing for an industrial chemist to work on.
More formally, the definition of a telescoped synthesis is 'A sequential 1-pot synthesis with reagents added one at a time without workup' which is what I described.
Now I was just guessing that a copper catalyst might be used but there is a ccommon amination methodology in which a base and a catalytic amount of NaI is used. The former obviously to neutralize the haloacid produced, the latter because a secondary chloro or bromo moiety will be swapped to the iodide in situ - and that's also cheaper than producing the alkyl iodide in the first place.
The exact details are, I'm certain, known only to the annointed few. But in real terms the price of MDMA has dropped. In the late 80s it was £100/gram for very pure product, 35 years later and it's £50/gram. So the only way someone can make a lot of money is to swap to very large scales. The sort of people involved are not the sort of people I would wish to associate with.
I'm pretty sure the name was changed because it's more accurate. You can have a vastly higher number of theoretical plates so it's possible to cleanly seperate componds with ALMOST idential MWs. A whole bevy of new types of chromatogrphy became possible as well.
Don't forget, the VOLUMES involved are tiny. Even if 1mL is at a HUGE pressure, it still doesn't contain much energy so doesn't represent much of a risk.
I am entirely guessing at what exact processes are involved, what I was trying to make clear was that there has been a huge paradigm shift. Even into the early 21st century there were people producing MDMA microcrystals and pilling them up on a vast scale. BUT moonrock entirely avoids the need to pill up the product - another saving. It's not a single improvement but freash eyes i.e. chemical engineers whose entire education is based on the idea that they will NEVER be dealing with a novel compound - that's medicinal chemist work. Chemical engineers look at how to scale a process and bing down costs.
A RT, solvent-free reaction that yields solid MDMA hydrochloride as the product would be an absolutely standard thing for an industrial chemist to work on.
More formally, the definition of a telescoped synthesis is 'A sequential 1-pot synthesis with reagents added one at a time without workup' which is what I described.
Now I was just guessing that a copper catalyst might be used but there is a ccommon amination methodology in which a base and a catalytic amount of NaI is used. The former obviously to neutralize the haloacid produced, the latter because a secondary chloro or bromo moiety will be swapped to the iodide in situ - and that's also cheaper than producing the alkyl iodide in the first place.
The exact details are, I'm certain, known only to the annointed few. But in real terms the price of MDMA has dropped. In the late 80s it was £100/gram for very pure product, 35 years later and it's £50/gram. So the only way someone can make a lot of money is to swap to very large scales. The sort of people involved are not the sort of people I would wish to associate with.
unodelacosa
Bluelighter
Yeah no shit ☞ they're not gonna state their duplicitous strategy to haggle insurance rates. And while I'm sure the primary driver of the shift from "pressure" to "performance" was technological advancement, it's highly plausible that risk mitigation and insurance considerations played a supporting role, especially as this is what's been indicated anecdotally. You yourself point out that cost cutting and efficiency are paramount to these companies. But now I'm the one speculating something unlikely to ever be known or provable. Time + discretion tend to do this.
Good point.
We all are. I'm not so sure it's useful being this exact in our conjectures though, at least for my part I'll say that. I'm enjoying reading your hypotheses nonetheless and you've brought up some interesting fresh things to ponder. Thanks for that!
Are you suggesting a paradigm shift in chemical engineering overall, a paradigm shift in the clandestine world, or do you think it's both, and if so, what makes you certain these shifts have influenced clandestine practices so quickly? I'm not saying you're wrong or that they haven't; I'm just curious your thoughts here and if any specific evidence influenced your thinking on this.
Arguably there's never been a need to "pill up" (or tablet-press) the product. Yes, I read the earlier comment about how pills were considered "cut-proof" until people started pulverizing them and repacking them either in new tablet punches or sometimes just in capsules as I recall seeing more than once. I think you're placing maybe too much importance on this marketing jargon "moonrocks" which is not always consistently applied, and I'll point out again that it ignores co-crystallizing agents and the aforementioned tendency for unscrupulous dealers to make shady moves in order to cut their product. Res ipsa loquitur.
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Are you sure that the batch you have sent to them is meh ?
ThreePointCircle
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Yep. Kinda depressing they didn't find anything.
I'm somewhat perplexed by the absolute absence of anything else. When you look at papers analysing samples they're always finding at least some levels of synth byproducts, etc... but this analysis showed nothing. Is it a threshold issue? I mean it's great that they've tested against that list, but if there are thresholds to it, that would be useful to know.
Edit: I mean, they should have at least found something, even if it was food colouring. It wasn't the cleanest looking batch ever.
4DQSAR
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What, you imagine that insurers don't know what they are insuring?
That would be unique.
I say again, the volumes of liquid that are under pressure are extremely small so a failure wouldn't result in some huge event.
If your just ignore volumes, I can equally point to other lab techniques that use pressures many orders of magnitude higher - but again, the volumes are tiny.
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I am very perplexed by it. So much so that I'm thinking about deliberately adding an impurity and sending it in.
ThreePointCircle
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Oddly the thought had crossed my mind. I was wondering about asking them if they can say what the sensitivity of each test is set to but I don't want to come across as someone who is desperate to try and prove a point.
4DQSAR
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I don't believe ANYONE is trying to hide the synthesis by subtle addition of impurities. If they wanted to hide the route - they would remove ALL impurities. But that would require extra work. Telescoping is all about reducing costs. Telescoping also makes the synthesis much simpler, so the 'cooks' who actually make the stuff are likely well paid, but they must know that sooner or later they will get caught.
But the people above them - they aren't taking as many risks. They just drop off precursors and cash and pick up product. Yes, someone could watch a lab but that exchange could take place somewhere else making it a hugely costly endevour to catch one limb of one group. The people at the top don't even touch product or precursors and the cash is often washed.
Anyone else notice those 'American Cnady Stores' that are turning up throughout Europe? £6 for some soft-drink you never heard of. THAT is one example of how money is washed. Those shops appear and disappear every 12 months or so - just long enough to wash money, not long enough for anyone to question why shops nobody ever visit are still showing huge profits. Maybe they are less common this year as it became widely known what they were doing. But there are still large parts of the economy that work in cash. Farming being a good example. Farmers still widely use cash even for large-ticket items.
At the end of the day, these people are making huge quantities of MDMA and it's the PRODUCT that is most likely to get them into trouble. If you imagine that the precursors aren't known, I think you are mistaken. You overestimate the resources available to the USD (for example). That's HOW they are defeated - they have a budget and if the way you work means stopping you is too costly, they don't.
But the people above them - they aren't taking as many risks. They just drop off precursors and cash and pick up product. Yes, someone could watch a lab but that exchange could take place somewhere else making it a hugely costly endevour to catch one limb of one group. The people at the top don't even touch product or precursors and the cash is often washed.
Anyone else notice those 'American Cnady Stores' that are turning up throughout Europe? £6 for some soft-drink you never heard of. THAT is one example of how money is washed. Those shops appear and disappear every 12 months or so - just long enough to wash money, not long enough for anyone to question why shops nobody ever visit are still showing huge profits. Maybe they are less common this year as it became widely known what they were doing. But there are still large parts of the economy that work in cash. Farming being a good example. Farmers still widely use cash even for large-ticket items.
At the end of the day, these people are making huge quantities of MDMA and it's the PRODUCT that is most likely to get them into trouble. If you imagine that the precursors aren't known, I think you are mistaken. You overestimate the resources available to the USD (for example). That's HOW they are defeated - they have a budget and if the way you work means stopping you is too costly, they don't.
I agree - manufacturers add impurities inadvertently.
I mentioned adding impurities deliberately to ThreePointCircle only as a way to test the testing service.
Apples and oranges.
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Meh vs mwah BENZOFURY 11 YEARS ago
Borax a well respected member on the hive posted this 11 years ago. Why 6APB succinate sucks but HCL is BOMB. With NMR lab testing
Borax a well respected member on the hive posted this 11 years ago. Why 6APB succinate sucks but HCL is BOMB. With NMR lab testing
4DQSAR
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That was always the problem with the benzofurans. One has to take the ring, perform a chlromethylation and from that produce the carboxamide. The problem is that you ended up with positional isomers so you didn't get a pure product.
Now INITIALLY the 'Benzofury' brand of 5-APB / 6-APB was the hydrochloride salt. Clearly someone had used partial crystalization (or whatever) to obtain the pure precursor. It's only when Chinese vendors figured out there was a huge market, figured out they could produce it at a much lower price and figured out that people were mostly OK with an impure product.
Grisham's Law in action.
Now INITIALLY the 'Benzofury' brand of 5-APB / 6-APB was the hydrochloride salt. Clearly someone had used partial crystalization (or whatever) to obtain the pure precursor. It's only when Chinese vendors figured out there was a huge market, figured out they could produce it at a much lower price and figured out that people were mostly OK with an impure product.
Grisham's Law in action.
Column Chromatography im told eitherway it's important of course to document and understand it is happening elsewhere.
Awesome work. This is what I’ve been wanting to see. They have described the compound as MDMA-HCl and its purity as 92%.
It begs the question, what is the remaining 8% made up of, because I read this as not showing any further elution peaks on the chromatograph, but how can that be if there is 8% of “stuff” also in there.
The way in which they have done it also seems arse about. Having a set list of potential (and let’s face it rather obvious) contaminants and trying to match them is not how I thought this type of analysis ordinarily was done.
Isn’t the goal to try and separate the various other constituents of the sample (beyond the MDMA-HCl) with chromatography and then for any mystery peaks which reveal themselves and appear to be present in a materially relevant proportion, to then attempt to identify that chemical with the add of mass spectrometry, NMR and the like?
There should be 8% worth of other peaks (trace substances and general noise aside) to investigate and there should be NO assumptions made as to what any of the potential chemicals contained within that 8% might otherwise be.
One other matter that I feel does tend to get overlooked is that not only was there this change to the myriad of pre-precursors from 2012 onwards but the European and Australian drug analysis reports also reported at around the same time, a significant shift from borohydride as the reducing agent of choice, to hydrogenation via palladium and then later platinum catalysts. This may mean nothing of course, but likewise it may not.
As for what is being employed to reductively aminate the ketone in 2025 is anyone’s guess!