What is wrong with the MDMA available today? - v2

[LucidSDreamr]

Well, (racemic) MDMA/MDA/MDE are still reductively aminated from MDP-2-P, aka: PMK for piperonyl methyl ketone. PMK-glycidate was just a technicality to avoid issues with customs when shipping from China to other countries. There are still chemists who will steam distill or press sassafras plant roots for the oil, vacuum distill the safrole to purity, isomerize it and convert it to the ketone intermediate (PMK) and then reduce per usual with ammonia, methylamine or ethylamine. It's not as though glycidates were at all a necessary part of the process beyond disguising the ketone for customs purposes.

It was my understand that piperonyl like compounds were too restricted (this the need for disguise) and natural derived sassafras oil were too limited and used up and that was the reason the glycidate was used to produce most of the stuff in existence.

 

[unodelacosa]

piperonyl like compounds were too restricted

Please forgive me if I seem pedantic here, but my inner the chemistry nerd wants to clarify that the taxonomy of "piperonyl-like compounds" is a bit of an umbrella term, as it were. "Piperonyl" comes from piperonal, an aromatic compound in its chemical structure, which in turn traces back to piperine, the alkaloid found in black pepper (Piper nigrum).

Disclaimer: As has been stated, this is for harm reduction in understanding the relevant points of modern MDMA production and how any potential impurities might harm someone. Per site rules, this will not delve into the details or teach anyone how to manufacture. It takes extensive education, academic or otherwise.

Piperonal (aka heliotropin):

Used in fragrances & flavorings, smells pleasing, similar to other aromatic aldehydes (e.g.: vanillin, 4-anisaldehyde, benzaldehyde). It's found in vanilla, dill, violets, and black pepper. As mentioned, black pepper's aroma comes from piperine which has a chemical similarity to piperonal—plus 9 carbons, 3 hydrogens & 1 nitrogen atom arranged like so:

Piperine


This can be synthesized from catechol, btw. For reference to spot the similarity, here's MDMA:

MDMA

The resemblance should be obvious, I think. So that's the "piper-" portion of "piperonyl." As to the "-onyl" suffix, this denotes an aldehyde functional group (here, from piperonal).

And so "piperonyl" refers back to the pepper plant and its chemical derivatives, linking its origin to the natural source and its aromatic qualities. However, for MDMA, piperonyl methyl ketone (PMK) is the showstopper. If it's not available to purchase (it isn't without a proper license), then producing it with its closest obtainable precursor is the next best thing. Sure, Cambodia destroyed a bunch of safrole-containing plants but that was like eight years ago. The rumor is: new plants have grown in new locations. All in all, chemicals like MDMA, amphetamine, GHB, etc. are too simple to prevent people from producing it entirely. MXE, LSD, & other more complex molecules are often quite outside the purview of many a clandestine chemist I would imagine.

and natural derived sassafras oil were too limited and used up and that was the reason the glycidate was used to produce most of the stuff in existence.

Well, starting from PMK-glycidate is easier than starting from a heap of roots & plant parts, which, broad overview ☞ have to be steam-distilled or pressed to get the oil out (should be ~7% volume by weight). Then, under a constant vacuum to lower the boiling point, safrole has to be vacuum distilled to purity from this crude plant oil. Safrole now obtained, it has to be gently refluxed and isomerized so it can be oxygenated into the ketone intermediate, MDP-2-P, aka PMK. That's a lot of steps compared to detaching the glycidate from Chinese PMK. Of course, junk in, junk out; so the initial PMK quality does matter. But anyway glycidates are easy to form with a base and remove with an acid. For example, benzyl glycidates can be synthesized by combining benzaldehyde with methyl chloroacetate under basic conditions. This reaction forms the glycidate structure via a condensation and cyclization process.

There are many precursor starting points for producing MDMA, such as the aforementioned heliotropin, but to your point, when one source became pinched, the clandestine world did what it does best and pivoted to a new source. In this case, the new source-precursor was Chinese PMK-glycidate, which had its "honeymoon period", so to speak, until law enforcement caught up in the ongoing cat-and-mouse game… that ship has sailed now. But the common denominator among these precursors is the basic structure, 1,2-methylenedioxybenzene, aka…

1,3-Benzodioxole:

Check out how many benzodioxoles and 4-phenylpiperidines there are in these lists:

• Benzodioxoles
• 4-Phenylpiperidines

EDIT: An added consideration is the fact that PMK has a short shelf-life, while PMK-glycidate is more stable.

 

[Didgital]

Please forgive me if I seem pedantic here, but my inner the chemistry nerd wants to clarify that the taxonomy of "piperonyl-like compounds" is a bit of an umbrella term, as it were. "Piperonyl" comes from piperonal, an aromatic compound in its chemical structure, which in turn traces back to piperine, the alkaloid found in black pepper (Piper nigrum).

Disclaimer: As has been stated, this is for harm reduction in understanding the relevant points of modern MDMA production and how any potential impurities might harm someone. Per site rules, this will not delve into the details or teach anyone how to manufacture. It takes extensive education, academic or otherwise.

Piperonal (aka heliotropin):

Used in fragrances & flavorings, smells pleasing, similar to other aromatic aldehydes (e.g.: vanillin, 4-anisaldehyde, benzaldehyde). It's found in vanilla, dill, violets, and black pepper. As mentioned, black pepper's aroma comes from piperine which has a chemical similarity to piperonal—plus 9 carbons, 3 hydrogens & 1 nitrogen atom arranged like so:

Piperine


This can be synthesized from catechol, btw. For reference to spot the similarity, here's MDMA:

MDMA

The resemblance should be obvious, I think. So that's the "piper-" portion of "piperonyl." As to the "-onyl" suffix, this denotes an aldehyde functional group (here, from piperonal).

And so "piperonyl" refers back to the pepper plant and its chemical derivatives, linking its origin to the natural source and its aromatic qualities. However, for MDMA, piperonyl methyl ketone (PMK) is the showstopper. If it's not available to purchase (it isn't without a proper license), then producing it with its closest obtainable precursor is the next best thing. Sure, Cambodia destroyed a bunch of safrole-containing plants but that was like eight years ago. The rumor is: new plants have grown in new locations. All in all, chemicals like MDMA, amphetamine, GHB, etc. are too simple to prevent people from producing it entirely. MXE, LSD, & other more complex molecules are often quite outside the purview of many a clandestine chemist I would imagine.


Well, starting from PMK-glycidate is easier than starting from a heap of roots & plant parts, which, broad overview ☞ have to be steam-distilled or pressed to get the oil out (should be ~7% volume by weight). Then, under a constant vacuum to lower the boiling point, safrole has to be vacuum distilled to purity from this crude plant oil. Safrole now obtained, it has to be gently refluxed and isomerized so it can be oxygenated into the ketone intermediate, MDP-2-P, aka PMK. That's a lot of steps compared to detaching the glycidate from Chinese PMK. Of course, junk in, junk out; so the initial PMK quality does matter. But anyway glycidates are easy to form with a base and remove with an acid. For example, benzyl glycidates can be synthesized by combining benzaldehyde with methyl chloroacetate under basic conditions. This reaction forms the glycidate structure via a condensation and cyclization process.

There are many precursor starting points for producing MDMA, such as the aforementioned heliotropin, but to your point, when one source became pinched, the clandestine world did what it does best and pivoted to a new source. In this case, the new source-precursor was Chinese PMK-glycidate, which had its "honeymoon period", so to speak, until law enforcement caught up in the ongoing cat-and-mouse game… that ship has sailed now. But the common denominator among these precursors is the basic structure, 1,2-methylenedioxybenzene, aka…

1,3-Benzodioxole:

Check out how many benzodioxoles and 4-phenylpiperidines there are in these lists:

• Benzodioxoles
• 4-Phenylpiperidines

EDIT: An added consideration is the fact that PMK has a short shelf-life, while PMK-glycidate is more stable.

Everything you say is true, but let's make sure any synthesis talk stays superficial.

The important part to understand, is that almost all MDMA, whether it's made from safrole or Chinese pre-precursors proceed through the intermediate, PMK. PMK is not racemic, so any mdma made from it shouldn't differ in enantiomer ratios though it's conceivable that PMK made from different sources could contain different impurities.

The other historic route is from piperonal, which requires nitroethane which is heavily restricted most places in the world.

 

[unodelacosa]

Everything you say is true, but let's make sure any synthesis talk stays superficial.

The important part to understand, is that almost all MDMA, whether it's made from safrole or Chinese pre-precursors proceed through the intermediate, PMK.

Outside of a few unconventional techniques using specialized equipment—like electrolytic hydrogenation—and a handful of low-yielding, obscure-ish syntheses to arrive at the target compound, you're right – reducing the intermediate ketone is the most popular route to MDMA.

PMK is not racemic, so any mdma made from it shouldn't differ in enantiomer ratios though it's conceivable that PMK made from different sources could contain different impurities.

So PMK-glycidate is racemic even though PMK is not. This could alter outcomes a bit, I think.

Also, commercially available PMK has been GC-MS tested and studied, and it was determined that some of the impurities included:

Impurity compound from legal PMK	Also known as / known for	Structure
3,4-Methylenedioxyallylbenzene	Safrole
3,4-Methylenedioxyphenyl-1-propene	Isosafrole
3,4-Methylenedioxybenzaldehyde	Piperonal, Heliotropin
3,4-Methylenedioxyphenyl-2-propanone-(3-ol)	3,4-Methylenedioxyphenylpropanol
3,4-Methylenedioxyphenyl-1-propanone	MDP1P, a methylone precursor
3,4-Methylenedioxyphenyl-1-butanone	MDP1B, an ethylone precursor
3,4-Methylenedioxyphenyl-propionic acid-2-one	a carboxylic acid, -COOH instead of -COCH₃

Those all have 3,4-methylenedioxy rings. These next two do not:

• 4-Allyl-1,2-dimethoxybenzene
• 4-Isopropyl-1,6-dimethyl-1,2,3,4-tetrahydronaphthalene

There was another good study done in 2004 that discovered even more impurities after mimicking popular clandestine routes of MDP-2-P production (via performic acid as well as via MDP-2-nitrostyrene intermediate using nitroethane).

The other historic route is from piperonal, which requires nitroethane which is heavily restricted most places in the world.

Yeah but piperonal goes to → MDP-2-nitrostyrene, which is very similar, and then on its way to the end product, I believe it passes through MDP-2-P. It's very nearly the same thing and serves the same function albeit with a different precursor, reagents, and catalyst.

Also, nitroethane isn't but so watched.

 

[Didgital]

PMK-glycidate is racemic even though PMK is not. This could alter outcomes a bit, I think.

Even if the glycidate is racemic the ketone loses no longer has a chiral carbon. Both S/R or D/L glycidate will oxidize to the exact same ketone. MDP2P as I like to call it.

 

[unodelacosa]

Even if the glycidate is racemic the ketone loses no longer has a chiral carbon. Both S/R or D/L glycidate will oxidize to the exact same ketone. MDP2P as I like to call it.

Absolutely, if everything is done properly. With clandestine chemistry, you never know. Analytics are often absent, and inexperienced workers make mistakes or neglect basic procedures. I'm thinking if the conversion yield from PMK-glycidate to MDP2P (as you like to call it) isn't 100%, then it's possible some of the glycidate makes it through to downstream reactions where its chiral makeup could potentially affect the end product in a stereoselective manner, though to what degree is unclear. You see what I'm saying? Although it likely doesn't matter; I was just musing.

 

[user666]

If the conversion of PMK Glycidate to PMK is not 100% efficient then some PMK Glycidate is left in the reaction vessel.
If this unreacted precursor is not removed completely by the subsequent workup, it can get amidated and its epoxy ring can be opened by subsequent reaction with Methylamine, generating M-ALPHA-HMCA as a contaminant.
A reaction with dimethylamine will produce another variant.

This is not a theoretical compound. It actually occurs in Molly pills, see this report.

The Lee paper investigated the M-ALPHA-HMCA chemistry.

Amide is a compound with the general formula R−C(=O)−NR′R″, where R, R', and R″ represent any group. Formamide is the simplest amide.

 

[vash445]

Outside of a few unconventional techniques using specialized equipment—like electrolytic hydrogenation—and a handful of low-yielding, obscure-ish syntheses to arrive at the target compound, you're right – reducing the intermediate ketone is the most popular route to MDMA.


So PMK-glycidate is racemic even though PMK is not. This could alter outcomes a bit, I think.

Also, commercially available PMK has been GC-MS tested and studied, and it was determined that some of the impurities included:

Impurity compound from legal PMK	Also known as / known for	Structure
3,4-Methylenedioxyallylbenzene	Safrole
3,4-Methylenedioxyphenyl-1-propene	Isosafrole
3,4-Methylenedioxybenzaldehyde	Piperonal, Heliotropin
3,4-Methylenedioxyphenyl-2-propanone-(3-ol)	3,4-Methylenedioxyphenylpropanol
3,4-Methylenedioxyphenyl-1-propanone	MDP1P, a methylone precursor
3,4-Methylenedioxyphenyl-1-butanone	MDP1B, an ethylone precursor
3,4-Methylenedioxyphenyl-propionic acid-2-one	a carboxylic acid, -COOH instead of -COCH₃

Those all have 3,4-methylenedioxy rings. These next two do not:

• 4-Allyl-1,2-dimethoxybenzene
• 4-Isopropyl-1,6-dimethyl-1,2,3,4-tetrahydronaphthalene

There was another good study done in 2004 that discovered even more impurities after mimicking popular clandestine routes of MDP-2-P production (via performic acid as well as via MDP-2-nitrostyrene intermediate using nitroethane).


Yeah but piperonal goes to → MDP-2-nitrostyrene, which is very similar, and then on its way to the end product, I believe it passes through MDP-2-P. It's very nearly the same thing and serves the same function albeit with a different precursor, reagents, and catalyst.

Also, nitroethane isn't but so watched.

Some of these have been talked about here but not others..

3,4-methylenedioxyphenylacetic Acid. 3,4-methylenedioxycinnamic Acid. Just about any 3,4-dihydroxy compound and an appropriate methylating agent. Grignard Reaction on 5-bromo-1,3-benzodioxole with an Allyl Halide. Friedel-Crafts with Allyl Chloride on 1,3-benzodioxole. Directly to the amine with N-Trifluoroacetamide (Alanine --> N-Trifluoroacetylalaninol --> N-Trifluoroacetylalanolyl Chloride --> Friedel-Crafts on 1,3-BDO, and hydrolysis) or Friedel Crafts with 2-chloro-3-methyl-1R-aziridine (which causes spontaneous ring-opening into the isopropylamine). bisulfate adducts

Switching from MDRA to 5-aminopropylbenzofuran or 5-aminopropylindane/indole.

Synthesis of R- and S-MDMA via nucleophilic ring-opening of homochiral N-tosylaziridines Homochiral (R)- and (S)-3,4-methylenedioxymethamphetamine (MDMA) were prepared in six steps (each) from the chiral pool precursors D- and L-alanine, respectively. The key step, copper-catalysed regioselective ring-opening of an N-tosylaziridine with an aryl Grignard reagent, proceeded in high yield with complete regioselectivity. Elaboration was achieved with preservation of configurational integrity, affording R- and S-MDMA hydrochlorides with enantiopurities of >99.5%, as determined by enantioselective HPLC with fluorescence detection. Attempts to apply the synthetic methodology to the synthesis of the homochiral enantiomers of the α-phenyl analogue of MDMA (UWA-001) were thwarted by a switch in regioselectivity in the key step.

Underground chemists have always adapted, and always will, and there are always greedy bastards willing to accidentally shamelessly break the law if there's profit in it.


MAMDPA; MDMAPA; methyl 3-oxo-2-(3,4- methylenedioxyphenyl)butanoate. MAPA MD twin cousin. Has seen to be talked about but has made watch lists recently.

methylenedioxyphenylpropane with dimethylcarbonate, then react product with hydrochloride methylamine and alkaline catalyst (like lithium diisopropylamide). Then react product of this reaction with sodium hypochlorite. Yield - MDMA hydrochloride ~ This synthesis requires careful control of reaction temperatures and stoichiometry due to the sensitivity of the intermediates involved.

3,4-Methylenedioxyphenylacetonitrile, Methylenedioxyphenylisobutyric acid , Dibromo or iodo compounds or azide compounds ... etc.

. The Pinnick Oxidation should take the aldehyde to 3-(1,3-benzodioxol-5-yl)-2-methylpropanoic acid. Then, the Hunsdieker will leave you with the bromopropane. The bromo propane being the very thing you could use to aminate or 'methyl-aminate' for MDA or mdma?

You can make Benzodioxole from catechol and Ch2Cl2.
Then react this with glyoxylic acid to get 3,4-methylenedioxymandelic acid.
Then to piperonal using O2 and CuCl2 or using AgNo3. Then to iso safrole






Personally i've always wondered about helional to piperonal to isosafrole. maybe via a PIPERONYL FORMALDEHYDE intermediate

images hosted at ImgBB

Image images hosted in ImgBB

ibb.co

 

[Didgital]

Some of these have been talked about here but not others..

3,4-methylenedioxyphenylacetic Acid. 3,4-methylenedioxycinnamic Acid. Just about any 3,4-dihydroxy compound and an appropriate methylating agent. Grignard Reaction on 5-bromo-1,3-benzodioxole with an Allyl Halide. Friedel-Crafts with Allyl Chloride on 1,3-benzodioxole. Directly to the amine with N-Trifluoroacetamide (Alanine --> N-Trifluoroacetylalaninol --> N-Trifluoroacetylalanolyl Chloride --> Friedel-Crafts on 1,3-BDO, and hydrolysis) or Friedel Crafts with 2-chloro-3-methyl-1R-aziridine (which causes spontaneous ring-opening into the isopropylamine). bisulfate adducts

Switching from MDRA to 5-aminopropylbenzofuran or 5-aminopropylindane/indole.

Synthesis of R- and S-MDMA via nucleophilic ring-opening of homochiral N-tosylaziridines Homochiral (R)- and (S)-3,4-methylenedioxymethamphetamine (MDMA) were prepared in six steps (each) from the chiral pool precursors D- and L-alanine, respectively. The key step, copper-catalysed regioselective ring-opening of an N-tosylaziridine with an aryl Grignard reagent, proceeded in high yield with complete regioselectivity. Elaboration was achieved with preservation of configurational integrity, affording R- and S-MDMA hydrochlorides with enantiopurities of >99.5%, as determined by enantioselective HPLC with fluorescence detection. Attempts to apply the synthetic methodology to the synthesis of the homochiral enantiomers of the α-phenyl analogue of MDMA (UWA-001) were thwarted by a switch in regioselectivity in the key step.

Underground chemists have always adapted, and always will, and there are always greedy bastards willing to accidentally shamelessly break the law if there's profit in it.


MAMDPA; MDMAPA; methyl 3-oxo-2-(3,4- methylenedioxyphenyl)butanoate. MAPA MD twin cousin. Has seen to be talked about but has made watch lists recently.

methylenedioxyphenylpropane with dimethylcarbonate, then react product with hydrochloride methylamine and alkaline catalyst (like lithium diisopropylamide). Then react product of this reaction with sodium hypochlorite. Yield - MDMA hydrochloride ~ This synthesis requires careful control of reaction temperatures and stoichiometry due to the sensitivity of the intermediates involved.


Methylenedioxyphenylisobutyric acid as mentioned above , Dibromo or iodo compounds or azide compounds ... etc.

. The Pinnick Oxidation should take the aldehyde to 3-(1,3-benzodioxol-5-yl)-2-methylpropanoic acid. Then, the Hunsdieker will leave you with the bromopropane. The bromo propane being the very thing you could use to aminate or 'methyl-aminate' for MDA or mdma?


There is so much stupid ahit on this thread I have no idea how to respond. I think most of you are.... if not idiots, then I think you have feelings that overpower logic and evidence





Personally i've always wondered about helional to piperonal to isosafrole. maybe via a PIPERONYL FORMALDEHYDE intermediate

images hosted at ImgBB

Image images hosted in ImgBB

ibb.co

 

[user666]

There is so much stupid ahit on this thread I have no idea how to respond. I think most of you are.... if not idiots, then I think you have feelings that overpower logic and evidence

What made you write that ?

 

[vash445]

What made you write that ?

probably because I put PIPERONYL FORMALDEHYDE intermediate, PIPERONYL FORMALDEHYDE is PBO and you cant use PBO for MDA/MDMA

To be fair I did say an intermediate of PIPERONYL FORMALDEHYDE not PBO directly my only guess...

However since synethsis discussion is not allowed. And it could very well later close a path I would rather not talk about them.

 

[Mr. Krinkle]

i have some that i haven't even tried yet


i need to get on it


(true story)

 

[Didgital]

probably because I put PIPERONYL FORMALDEHYDE intermediate, PIPERONYL FORMALDEHYDE is PBO and you cant use PBO for MDA/MDMA

To be fair I did say an intermediate of PIPERONYL FORMALDEHYDE not PBO directly my only guess...

However since synethsis discussion is not allowed. And it could very well later close a path I would rather not talk about them.

wtf are you even talking about. I would delete your post if it actually resembled reality. No one is doing that anyway... I'm biting my tongue here as a mod.

What made you write that ?

Lets just say that all of these precursors eventually move through PMK so it doesn't matter what your starting source is, your input prior to MDMA is PMK which is not racemic, so if you go safrole to pmk vs some pre-precursor, youre still going through the same intermediate. I would advise you to pretty much delete this entire thread from your data bank. It's either old heads reminiscing or people who have no idea what they talking about that love to theorize. And when you present them evidence, it doesn't matter. They unwilling to change their belief system at this point. So why bother trying to change them/views.

I just pop in every once in a while to make sure the synth talk doesn't get too detailed.

Hate this thread. I see it as a purveyor of misinformation more than anything else. Good clean MDMA is available.... (Pro tip don't buy drugs from someone on the street, not that that's a pro tip)

I'm willing to bet vast majority of commenters here have never made MDMA in their life and while some here do have some chemistry knowledge, they look for answers that validate their claims instead of using the scientific method. (WHAT THAT GC ANALYSIS SAID ITS MDMA?! THEY MUST NOT KNOW HOW TO LOOK"


Armchair chemists mostly.

 

[Mr. Krinkle]

don't close this thread

@unodelacosa isn't an idiot either


in fact, im glad he's here and i think he maintains this thread better than anybody else

 

[vash445]

wtf are you even talking about. I would delete your post if it actually resembled reality. No one is doing that anyway... I'm biting my tongue here as a mod.

piperonyl isobutyrate vs Piperonylidene propionaldehyde vs piperonylidene acetone

Visually at a glance...

I found a few others. But haven't spent the time to actually break it down

 

[vash445]

WHAT THAT GC ANALYSIS SAID ITS MDMA?! THEY MUST NOT KNOW HOW TO LOOK"

I'm saying I've done 3 labs that use GC/MS all tested 98- 99% pure. (for they NAYSAYERS that it's impossible due to the HCL salt binding) YES YES, WE KNOW we are talking of " Freebase" purity... Not the difference between HCl, Sulphate or succinate form etc etc, We are saying EC and others including uni labs just report MDMA via GC/MS...

Same samples sent via NMR and GC/MS MALDI also tested as the MDMA mol weight...
At uni lab we as a group here of course... noticed discrepancies on only NMR detected. Is this always the case. Maybe not. But I'm just saying 2-3 labs GC/MS tested good.

All MDMA failed NMR but 1 magic batch. And found impurities other labs missed including a lab that checked GC/MS, then MALDI, then NMR after... if anyone wants to argue that, we need more NMR graphs of both MEH and magic. I mean at least to start...

Personally I feel issues have been 2 fold

1) chemists have not been distilling freebase oil. Or mdp2p and not distilling, when also not use bisulfate could also be then causing side products then occur. This artificially bulks product and labs view it as "noise" without graphs it's all "fluff" so to speak

2) most labs I heard titrate and not use HCL gas. This is just a theory.

Yes there is good MDMA there is also bad in my exp. I'm not saying they don't know how to look. But it would help if we had GC/MS HPLC and NMR and possibly XDR. And the graphs to back it up.

I DO also know, I once thought I had nitroethane OTC.. GC/MS I think said it was good. Failed a Henry and NMR... that alone should tell you how much to trust GC/MS alone... (Granted these are personally musings, I've encountered.. I could be lying right... but why would I?) Like everyone here I want to get to the bottom, and putting purposely BAD info is probably worse then NO INFO. And of course purposely bad info is different then miseducated info. Remember even attorney's argue about the law in front of a judge, Just like a scientist would argue for or against "flat earth" like Aristotle did. At least NOW we don't risk being either called a witch or a crackpot theorist when we may have different views... let alone risk being burned at the cross ,or exiled from Athens for criticising the government even if we were right or wrong eventually

For example anyways... OTC NE later via NMR showed. 1-Nitropropane (1-NP) AND 2-nitropropane OR SOMETHING similar came back. Unlike with GC/MS said confirmed NE...

I later did find confirmed nitroethane, and safrole NMR confirmed.

I will also say if I WAS EVER BUSTED. And I felt I had meh... I would argue it's potentially an analogue or something and require HPLC and NMR if I was fighting a law case....

P.S. Luckyduck also once offered a $10K BOUNTY on his NMR Xanax API powder, he had one done he wanted a second one,,, I asked why no GC/MS or even HPLC... they stated, I've had issues in the past when they claimed it was pure, it was not I then took a "yellow" xanax powder from a new vendor to EC as licking the powder was not bitter, was not diluting right, in pure ethanol or PG juice.. With EC GC/MS results as "99%" pure, I assume it was "pressing powder" as it came back 99% pure via EC ( I did not have access to NMR back then either like we do know) . However even with a slight tolerance back then, I did eventually have multiple red flags popped up, people said it was impure/ no effect when diluted from this new vendor.. Hence why, I really don't like "Just GC/MS" anymore... And defiantly see his point now... considering how it was 99% binder and 1% presumed xanax at this point... Granted, I could be lying... but to me seems pointless. And partially why, I don't take GC/MS readings to face value anymore...

 

[vash445]

I'm willing to bet vast majority of commenters here have never made MDMA in their life and while some here do have some chemistry knowledge, they look for answers that validate their claims instead of using the scientific method. (WHAT THAT GC ANALYSIS SAID ITS MDMA?! THEY MUST NOT KNOW HOW TO LOOK"


Armchair chemists mostly

Here is what I will say to being an "armchair"

I by NO MEANS hold any degree in chemistry either analytical, O-chem, bio synth with a crispr, etc etc. But I can read and decipher MOST patents. Some just go WAYYYY over my head also and some that go overhead I get like 50%.

I like maybe many others got A LOT info learned from TS2 AND HIVE. Strike always said this is a base, a MAP AND COMPASS not many people headed his words. Yes I do have plenty of safrole and NE if I want it all OTC by in large no waivers. Yes If I wanted to I could also start from piperonal acetate or the alcohol or other unlikely watched products. I got a very nice cop and judge that let me go with a stern warning and me being watched. Mainly because the claim was "explosives" which HELL NO I wouldn't ever do and with hexamine but no nitric acid they had a weak case. But alas. That helped beat my case. Reguardless I STOPPED ASAP being too watched however. You also price wise by in large can't beat the super duper labs. Especially all the risk considered... have spoken to MANY MANY people who do hold Masters of chemistry degrees in either O chem or analytics and they go you are better then the class I teach... Anyways does this mean I know everything? Hell I can't even get nomenclature or smiles correct half of the time. For me to calculate Avagadro's number or mols it would take me A WHOLE lot longer then I would like to admit it would take me to solve because.. I haven't done it in ages..

However, there is usually as I discussed earlier 3 levels of lab people.

1) people who read recipes and do monkey see monkey do "bath tub labs" They are the LOW end of the rung willing to make as much product sloppy in the preview of profits. These labs probably typically use glycidate and I'll call these monkey see diy pancake mixers. Maybe just 1 step up from DMT extraction so to speak. As the glycidate is soupfonicaion like the extraction of deemz by in large. I assume people will call this champagne and while there are "rocks" the chemical bonds are weak and break down to powder. My understanding the crystal structure is not "right"

2) the mid level guy. The mid level guy is someone who has a MUCH MUCH deeper understanding of chemistry. They took TS2 AS A map and compass or have a degree. And with enough time either develope their own less likely watched paths by doing some funny work. Either via glycolic acid or even better more off the "beaten path" as I've described coming up with something unique more unique the acetate or similar routes but there's others LESS WATCHED of course... That second part isn't too hard with a little effort and work, and reviewing patents and adapting but you have to be pretty fucking deep into chemistry. Their purity may or may not be better then #1 but they don't just blindly follow a recipe that happens to have mols or something miscalculated... They confirmed their work, may have access to safrole, etc. These people CANNOT COMPETE WITH #3 the pickards and Nick Sands etc of the world.. they MAY or may NOT have chemistry degrees. But even so, lab work is different then arm chair theory ... so to speak.

3)
Anyone can make pancakes user #1. Anyone with enough time can make their own pancake mix with their "special" sourdough or buckwheat starter we will call these usually between #2 and #3. However, the difference between someone following a recipe, someone making their own mix and someone (making, eggo waffles/pancakes or poptarts for Kellogg's doing chemical engineering) a #3 lab are 3 different skills. And I believe that is where we are at. Remember even Kelloggs, etc get recalls from either contaminated batches, misprinted pucks or chips etc etc. This is a LEVEL where even #1 or #2 can't compete of SCALE Period. At this point I'm assuming it's 55+ gallon jacketed reactors or alike. They might create a new route for fun, either for greater, yeild, less side products, or just experiment more then a #2 for "fun". These guys might have ugly looking grey rock stuff. But it was chemically bonded where even a hammer couldn't break it easy and was some pure FLAME as MDA. As Gale said I can't account for the blue color. But it is quite good amazing purity actually...

The path for a molecule, therefore, from early-phase API and drug product to a commercial product, is an iterative one. It involves increased levels of understanding around the synthesis, potential impurities, isomers, crystalline forms, and physical properties—all of which need to be controlled and understood to the fullest, as they can have an effect the safety and pharmacology of the drug.

The chemistry of MDMA is not a given, and requires expert development to get to the commercial standard we need to ensure patient access and safety at scale. However, it should not be expected that we will stop learning about the chemistry of this compound; changes in manufacturing process, scale, and product formulation can bring with them new challenges and lessons.

These are mechanics of chemistry that while anyone can make bathtub MDMA or meth.It takes someone true understanding not only the synthesis but how to also chemically manipulate the bonds.

To go from 94% to 99% is reallly hard. Hell I purified white stuff, removed purple junk from WHITE MDMA. Made crystal clear MDMA that looked like shards of meth so clear you could see thru it. It was still meh MDMA and tested as MDMA but was VERY lack luster. This MDMA made both BEAUTIFUL flat prisms and square cubes. They were bonded as TRASH. Very easy to break.

My only guess is I live in an extremely high humidity area and had water contimation via recrystallization due to high humidity. Recrystallization was done with 99% + dry ethanol, 99% methanol and isopropyl and 99%+ dry acetone and Dh20 , Ethyl acate was not tried yet... These were FRESH non opened bottles as well... Part of me wondered if I should have either distilled again just in case.. or use a molsieve... Reguardless

If I could I would try again I would probably use pressure/heat recrystallization next time instead.


Anyways I had the person ask me these questions help teach me to make man.... He asked, How detrimental is the 5-6 percent really when asked is there much of a difference. There are the Walter White's and Gales of the world. There is also Gus fringe "How pure can pure reallly be" I said you should learn to purify your own before you start running boy...

Gale mentions the blue meth that Gus had him test. He tells Gus that his own meth is 96% pure, a hard work and HARD EARNED but this blue meth is 99% pure. Gale says there's a huge difference between the two and that Gus should hire whoever made the blue meth. Gus says for our purposes 96% is just fine. Gale goes. It might not seem like it's a lot but it's a lot. It's Tremendous!

Yes, the basic chemistry is clod-simple, or at least as close to clod-simple as organic chemistry ever gets. You can, if you're of a mind to, learn how to do it in an hour. I've done more complex experiments in a high school chemistry class that I failed.

But the devil, as they say, is in the details.

There is a difference between running a reaction in a beaker when you're sitting there with your goggles and your lab coat babying it, and doing it at production volumes. Even a simple reaction becomes a whole ‘nother world when you're doing it repeatably on an industrial scale. It's the difference between a notion of water and an ocean of water.

Doing it is just chemistry. No, scratch that, it's not even chemistry, it's following a recipe. Can you make pancakes? Then you have what it takes to cook meth, other than the difficulty in sourcing the chemicals.

Doing it on the scale that was in the TV show as reliably and with the level of quality control they showed on the TV show is not chemistry. It's chemical engineering. Chemical engineering is neither simple nor easy. Chemical engineering is a combination of chemistry, process management and control, mass production, manufacturing, and engineering design (and the chemistry part is not necessarily the hardest part).

I believe Jessie Pinkman, when hired by the cartel in mexico and told to work talks about what about. If there is excess humidity in the room ,what will you do. That goes back to polymorphs and hydrates debate. Without the right equipment.

There are 3 anhydrous and 4 hydrates of MDMA. DO YOU KNOW if you have form 1,2 or 3... or do you know if you have 1 of the 4 HYDRATES? I bet you dont... Do you have a XRD to test which form or hydrate you have? This of course goes back to talks of

For over 100 samples, only one sample was found to contain anhydrous MDMA·HCl. This seized sample had a peculiar appearance as a very fine and dusty powder. It is noteworthy that re-analysis of this particular sample a year after seizure showed that the MDMA·HCl transformed into its hydrated state as described for model substances in section 3.5. The rareness of anhydrous MDMA·HCl is also depicted in Fig. 8, where an overlay of randomly selected casework samples (2019 – 2020, The Netherlands) showed that all crystalline samples (Fig. 8, B) and all tablets (Fig. 8, C) show the spectral features diagnostic for hydrated MDMA·HCl in their NIR spectrum.


Thorough polymorph screening is crucial in the understanding of active pharmaceutical ingredients as different polymorphs may exhibit variations in solubility, bioavailability, stability, and other critical properties in the evaluation of a drug. (1,4,10,11) There are many techniques to induce crystallization for polymorph screening including antisolvent methods, solution-based methods, evaporation methods, high-pressure crystallization, and crystallization from the melt. (4,11−20) While many recent studies on ritonavir relate to its performance as an amorphous solid dispersion, there have been recent advances in understanding the crystallization of ritonavir. (4,21−25) After the appearance of Form II ritonavir, two new solvates and an anhydrous form were discovered by Morissette et al. (4) In 2014, Kawakami et al. published their findings after crystallizing ritonavir from its melt. They detected the appearance of a crystalline form after annealing in a 60 °C oven over a period of several days. (24) They concluded that the material was Form IV identified by Morissette et al. (4,24) However, the X-ray powder diffraction (XPRD) patterns labeled as such do not match the Form IV XRPD pattern in the publication by Morissette et al. (4,24)

https://www.sciencedirect.com/science/article/pii/S2468170922000674

The path for a molecule, therefore, from early-phase API and drug product to a commercial product, is an iterative one. It involves increased levels of understanding around the synthesis, potential impurities, isomers, crystalline forms, and physical properties—all of which need to be controlled and understood to the fullest, as they can have an effect the safety and pharmacology of the drug. As someone who I would say I'm between a 1-2. But people with masters would probably say I'm a solid #2. I don't know the school knowledge to become a #3. My old friend who graduated west point for chemical engineering... and worked at military gov and Kelloggs yeah he probably could if I pried. But I would never ask him these questions....

Remember even in a SUPER LAB. GALE got like 95-96, it took Jessie a awhile to match GALES purity, when he got hired, and later Jessie under stress only reached like 60% consistently and Lydia got pissed and wanted walt back to get things on track. But to reach GMP 99.5+% PURE. CONSISTENTLY with the correct polymorph is no simple chemistry even ritonavir fucked up too many times. And then even found a new polymorph like years later after disaster #1. Ritonavir Form III is a new polymorph of ritonavir, an antiviral drug used to treat HIV/AIDS. It was discovered in 2023 through melt crystallization.
Properties of ritonavir Form III
Stability: Form III is the least stable of the three known polymorphs of ritonavir
Density: Form III is the least dense of the three polymorphs
Conformation: Form III has a different conformation than Forms I and II
Hydrogen bonding: Form III has different hydrogen bonding motifs than Forms I and II
Nucleation: Form III nucleates in a narrow temperature range of 60–70 °

 

[user666]

There are 3 anhydrous and 4 hydrates of MDMA. DO YOU KNOW if you have form 1,2 or 3... or do you know if you have 1 of the 4 HYDRATES? I bet you dont... Do you have a XRD to test which form or hydrate you have? This of course goes back to talks of

The crystalline forms of racemic 3,4-MDMA.HCl do not make any difference after complete dissolution in water because dissolution destroys all crystalline structures. The alternative pharmacological profile is manifested even after consumption of such solutions.

I welcome your musings about contaminants from improperly purified intermediate steps making their way to the final product but please stop the stuff about crystalline polymorphs of the final product.

 

[unodelacosa]

1) chemists have not been distilling freebase oil. Or mdp2p and not distilling, when also not use bisulfate could also be then causing side products then occur. This artificially bulks product and labs view it as "noise"

2) most labs I heard titrate and not use HCL gas. This is just a theory.

I agree, @vash445 – I've suspected for a while that chemists aren't bothering with vacuum distilling the ketone or the final product drug oil, nor are they cleaning the ketone whilst checking it with sodium meta bisulfite. And I also suspect they don't gas the end product but make an aqueous solution of drug + hcl acid and then they let it evaporate and call it a day without even an acetone rinse, let alone recrystallization. The reasons for doing this are obvious – it's easier and results in more "product" even at the expense of their product's purity.

I have to agree w/ @user666 that the crystalline polymorphs shouldn't matter if the purity is the same. That said, I understand the ways in which crystallography and crystallization itself is a purification technique, but I find it hard to believe it would have such an impact as to explain mythical meh MDMA.

I like maybe A LOT of other learned from TS2 AND HIVE.

Shout-out to Hobart, Rhodium, Spitball, OptimusPrime, Eleusis, Bandil, MethylMan, DrDrool, VibratingLights, and the other hive bees from the land of milk and honey…

 

[Didgital]

Shout-out to Hobart, Rhodium, Spitball, OptimusPrime, Eleusis, Bandil, MethylMan, DrDrool, VibratingLights, and the other hive bees from the land of milk and honey…

That's one thing I can agree on.

You forgot nicodem from science madness