Sciencemadness Discussion Board - What is wrong with MDMA production nowdays?

Nah I did methyl-j, and it feels totally different, but even better than MDMA, no way someone can mistake that for it.

I got arrested once for possession of xtc tablets.they were mbdp or methyl-j which is far superiority to mdma but the lab report said it was mdma.so whether they ran a gcms or whatever and knew it was mbdp and just ran with the mdma cause they could or they only confirmed it was a md amine of some sort of if they didn't do more than a presumptive feild test i don't know.and a few wks ago they found 700kgs of mdma and said it's the purest they've ever seen.

draculic acid69 - 13-1-2020 at 02:05

My pet theory is still that old ecstasy was spiked with amphetamine (duration 3-6 hours) and today's ecstasy is either not or it's got methamphetamine (duration 10-20 hours). Methamphetamine's half-life is mismatched with MDMA which makes it a poor adjuvant, but it's more likely to be synthesized in clandestine labs these days than regular old d-amph.

In my country ppl stopped adding meth to pills when mdma became cheaper than meth 13 yrs ago.around the same time as psuedoephedrine became hard to get.and while there was always ppl mixing mdma and meth in xtc pills it wasn't more common than 'occasionally happened'.

pastor - 13-1-2020 at 13:25

Quote: Originally posted by j_sum1

You say that it has the same profile as MDMA in gas chromatography mass spectroscopy. You also say that you have identified the product as racemic (although you did not mention how). Your third test is anecdotal physiological effect, which is really insufficient for any kind of conclusion: although it has caused you to raise the question. A scientific approach requires you to be a lot more systematic than swapping stories.

Logically your next step is NMR.

Not only testing companies were involved but also private labs. I'm reporting their findings.
NMR has been done, check it here: https://www.bluelight.org/xf/threads/what-is-wrong-with-the-...

Quote:

A "meh" sample was submitted for testing. The testers ran NMR 1H and 13C along with MALDI.
The MALDI came up 193.25 g/mol the mol weight of MDMA.

This batch of MDMA is a mixture of something that has practically the same NMR spectra as MDMA (both 1H and 13C) which means it has to contain the same carbon backbone and the same structural features, it cannot be an isomer because there are no isomers of MDMA which have the same mass and the same NMR spectrum.

1H NMR showed the issue on peak 9. Also, there is a mini peak at 207. Perhaps an an aldehyde or ketone. Overall, the sample has carbonyl impurities. The structure seems very close to what MDMA should look like in NMR but not quite.

@Assured Fish

Quote:

Do you really expect us to believe you have put together a culmination of reports where people have taken street drugs and analytically analysed them to find them all relatively pure before ingesting and accurately recording data on the effects.
If i didn't know any better id assume this as another exotic ploy to get us to spill our dirty little secrets on how to make drugs.

Many individuals has gotten their substance analyzed by the many companies that does substance testing, both european and north american.
range of purity (from what i can recall, it's a 180 pages long thread) is from 85 to 95%.
You can check the bluelight thread if you want.
there's plenty of info around (including here!) on how to make mdma, not my goal.

karlos³ - 13-1-2020 at 13:48

There is no way that some enantiomer mixture is achieved, it is either racemic(always) or enantiopure(never).
The only people who resolve enantiomers are curious home laboratorists.
And their produced enantiopure compound never makes it on the black market.

In short, be it safrole or the glycidate, MDMA is always made from piperonyl ketone.
So it should not differ at all from each other.
I even know people who got other routes to work(i.e. the halosafrole one), but it is just the same of course.

My opinion is, these are just plain urban myths, as the usual drug users do spread for most of the time, simply because they don't know better.
I don't give a damn about their unverified ramblings.

[Edited on 13-1-2020 by karlos³]

j_sum1 - 13-1-2020 at 14:19

Let's see if I have your story correct.

Here are a bunch of lab results from an assortment of samples of unknown origin. (They are all bona fide. Honest.)
Here are pages of uncorrelated anecdotal evidence on a message board.
My junkies are unhappy.
Guess what crap is in the pills.

OldNubbins - 13-1-2020 at 14:34

This is the hardest "two trains leave a station" problem I have ever seen...

Tsjerk - 13-1-2020 at 15:15

Do I really want to tell this? Probably not, but everyone probably already knew anyway so who cares...

These "MDMA pills are getting different" stories are bullshit. I have used a lot, weight out a lot for other people and have seen a lot of different reactions to the compound. After many usages the user does respond differently. I don't even consider taking it anymore, I only experience the (negative) side effects nowadays, no way around it.

First time? 80 mg is nice and fun and everyone is in heaven, second time, 90 does the same. After thirty times better take something else, because yes, you fried your brain. Doesn't have to be bad, but you did fry your brain. There is a Dutch case of a guy taking 3000 mg a day for ten years, just to stay normal. In the end he was normal.. You get used to about anything and MDMA is one you get used to easily.

Summary: it is your mind telling it could always be so good. A minor spike on a NMR spectrum is an impurity, and not a active one.

"Hey yer Honor Man...."

sodium_stearate - 13-1-2020 at 18:26

I only did acid like 22 times....

Ah, twice.

brubei - 14-1-2020 at 03:58

in another way... as i know, different polymorphism tend to yield in bioavailability issues. (https://www.sciencedirect.com/science/article/pii/S209580991...)

If we assume that new synthesis give new byproducts and maybe new polymorphic crystal, this may change some things...

need more data.

Tsjerk - 14-1-2020 at 05:05

Quote: Originally posted by brubei

in another way... as i know, different polymorphism tend to yield in bioavailability issues. (https://www.sciencedirect.com/science/article/pii/S209580991...)

If we assume that new synthesis give new byproducts and maybe new polymorphic crystal, this may change some things...

need more data.

That is for poorly soluble compounds. MDMA dissolves like a charm in the stomach and after that all crystal structure is gone.

This compound is structurally as simple as it gets... I really don't believe it would be missed if something really changed.

brubei - 16-1-2020 at 02:17

indeed

That's the deal with unregulated products, Also when speaking with drug users, everybody is saying that "things have changed". At any time.

SWIM - 16-1-2020 at 11:56

Quote: Originally posted by brubei

indeed

That's the deal with unregulated products, Also when speaking with drug users, everybody is saying that "things have changed". At any time.

Very true.
And not just drug users.

My great-grandmother always insisted that deer meat just don't taste the same anymore.

She blamed the advent of jet aircraft.

She and many of her old pals insisted that the noises jets make scare the animals and make them taste bad.

People can get mighty creative justifying their disappointments.

I once tried suggesting to her that the deer that she was shooting in her back yard probably didn't quite have the same diet as the ones she used to get in the woods, but she insisted it must be those durned jets.

(She was like 90, and couldn't get around too well anymore, so she'd leave kitchen scraps out for the deer, and shoot one every month or so.
She'd brace her gun against the wall to shoot, and she'd drag it up on the porch with a rope to butcher it. )

karlos³ - 16-1-2020 at 13:13

Well, but high levels of stress hormones really make meat taste bad, and deer is easily scared.
Your great-gram might be onto something there.
Of course, diet matters a lot too.

Nonetheless, your great-gram sounds like quite a women

[Edited on 16-1-2020 by karlos³]

draculic acid69 - 17-1-2020 at 00:26

Still shooting and butchering deer at 90 is pretty impressive

chemist1243 - 17-1-2020 at 05:43

its probably due to the formation of optical isomers which have slighlty different effects. for example, you can buy
levo-MethAmphetamine at any drugstore without perscription for around 3 dollars. even though its physical properties are exactly the same as Methamphetamine, its isomerism still exibits differnt effects.

karlos³ - 17-1-2020 at 06:03

Quote: Originally posted by chemist1243

its probably due to the formation of optical isomers which have slighlty different effects. for example, you can buy
levo-MethAmphetamine at any drugstore without perscription for around 3 dollars. even though its physical properties are exactly the same as Methamphetamine, its isomerism still exibits differnt effects.

It is either racemic or chiral, not something in between.
No one makes chiral MDMA, too expensive and requires too much effort, while providing a inferior product.
It is always a racemate.

G-Coupled - 17-1-2020 at 15:39

Quote: Originally posted by chemist1243

It is either racemic or chiral, not something in between.
No one makes chiral MDMA, too expensive and requires too much effort, while providing a inferior product.
It is always a racemate.

What about the ratios - is it 50/50? And if so, is it always?

clearly_not_atara - 17-1-2020 at 19:03

Yes, a chiral compound produced from achiral precursors will always have a near exact 50:50 ratio of isomers because there is nothing that can break the symmetry:

http://en.wikipedia.org/wiki/Symmetry_breaking

Usually this is the case with MDMA production because the chiral center is fixed in the last step (reductive amination) unless the bromosafrole technique is used, in which case the chiral center is fixed when the carbanion is protonated. Enantioselective catalysts or exotic precursors are necessary to achieve enantiomerically enriched ecstasy.

The one other thing I can think of is that if MDMA is produced by methylating MDA (particularly via the benzaldehyde/MeI method) it's possible that some amount of MDA would remain in the final product and affect the experience. This could be unintentional and may result in a stronger experience than MDMA alone. The assays you've provided have low confidences e.g. 85% purity which leaves plenty of room for an error like this.

[Edited on 18-1-2020 by clearly_not_atara]

stoichiometric_steve - 23-1-2020 at 23:22

Is everybody skimming over the fact that...i'm transforming into an idiot?

But seriously, how can MDMAs neurotoxicity be ignored here? Your users' anecdotal reports of declining quality may very well just be, like Tsjerk already said, effects related to neurological injury from regular use, quite possibly exacerbated, but most likely not attenuated by polytoxicomanic behaviour.

As long as you don't provide full substance profiling of the good ol' stuff vs the meh new stuff, including analysis for synthetic pathway specific impurities, where do you think this discussion is gonna go other than into a torrent of pure and ultimately meaningless speculation?

I mean, look at this:

Quote: Originally posted by chemist1243

its probably due to the formation of optical isomers which have slighlty different effects.

Quote: Originally posted by G-Coupled

What about the ratios - is it 50/50? And if so, is it always?

It's always 50/50 in racemic syntheses and never 50/50 in asymmetric syntheses. You could have known that if you had wanted to.

[Edited on 24-1-2020 by stoichiometric_steve]

pastor - 25-1-2020 at 09:59

2 new NMR were posted. The file ending ...207.pdf is confirmed magic, and the file ending ...579.pdf is confirmed meh.

On page 37 onwards there are reference 1H NMR plots.

The magic sample (...207.pdf) seems to match the reference MDMA HCL in D2O (page 45)
The meh sample ( ...579.pdf) appears be closest to MMDA base in CDCl3 (page 44). Not a super close match but I think its the best on my initial look
The other meh sample (...312.png) perhaps is also closest to MMDA but even less good a fit

So the big differences in the <7ppm range are: magic - peak around 4.87 (missing integration value?) that is not present in the meh sample. meh - big peak around 3.70 that is missing from the magic sample.

MAgic sample...

https://www.bluelight.org/xf/attachments/20200120115844207-p...

Meh sample #2
https://www.bluelight.org/xf/attachments/20200120174950579-p...

pastor - 25-1-2020 at 10:03

stoichiometric_steve It's def not excessive use, because we LITERALLY change batches and BAMB it's hits us.

MDMA virgins, drug virgins, Heavy users....

So it can't be effects related to neurological injury from regular use, quite possibly exacerbated,

[Edited on 25-1-2020 by pastor]

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Texium - 25-1-2020 at 10:29

@pastor: Could you please repost the NMR data directly in this thread? I would like to take a look at it, but I don't want to make a Bluelight account.

Sigmatropic - 25-1-2020 at 10:38

4.87 seems close to residual solvent signal of D2O, could be shifted due to pH effects of the ammonium salt. 3.7 in CDCl3 could be the NH on the amine itself. Can you attach them as a PDF? I'm not going to register at some site just to take a look at the NMRs. Also remember NMR is only sensitive to about 1% impurity so it's not going to tell you much.

clearly_not_atara - 25-1-2020 at 11:38

Sigmatropic: that's a really big peak for a residual solvent signal.

What I can say is that those two NMRs show different compounds :p

EDIT: the following analysis should have the warning that reading NMR is not exactly my strong suit

If I were to guess, the peak at 4.9 is the benzodioxole O-CH2-O shift. A carbon alpha to an ether increases the chemical shift from 1 to 3 ppm so at an acetal you might see something around 5 ppm. It's pretty rare for any moiety to have a peak here -- the only other thing is an alkene, which shouldn't be present. The high peaks are the aryl hydrogens.

Moving forward with this theory, the absence of the 4.9 peak in the second sample indicates that the "mehDMA" does not have a benzodioxole ring. Based on the descriptions of effects and the ability to simulate MDMA on test kits I suggest that the mystery compound is something like 3,4-dimethoxymethamphetamine. The "extra" peak around 3.7 is consistent with a phenolic ether, methinks.

Possibly, compounds like this are being introduced into the ecstasy supply by high-volume drug traffickers because they are cheap to produce and known to fool colorimetry.

[Edited on 25-1-2020 by clearly_not_atara]

karlos³ - 25-1-2020 at 11:57

This reminds me so much of drug users who speculate again and again if their meth contains either this benzylamine derivative or "it could be 4-MAR bruh!", when it is either bad or good...
They just talk shit and know nothing.

pastor - 25-1-2020 at 15:34

Quote: Originally posted by Sigmatropic

4.87 seems close to residual solvent signal of D2O, could be shifted due to pH effects of the ammonium salt. 3.7 in CDCl3 could be the NH on the amine itself. Can you attach them as a PDF? I'm not going to register at some site just to take a look at the NMRs. Also remember NMR is only sensitive to about 1% impurity so it's not going to tell you much.

4.87 is the residual solvent signal of D2O i'm told by the NMR...

That 3.7 is what is a huge mystery thou and is in BOTH meh sample MDMANMR and file 78985

[Edited on 25-1-2020 by pastor]

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pastor - 25-1-2020 at 15:52

Quote: Originally posted by Texium (zts16)

@pastor: Could you please repost the NMR data directly in this thread? I would like to take a look at it, but I don't want to make a Bluelight account.

all 3 NMR uploaded, ill look for the extended 13c on the VERY first MDMA meh sample I know we ran 1H and 13c

[Edited on 25-1-2020 by pastor]

karlos³ - 25-1-2020 at 15:57

What atara says has hand and feet.
It is not MDMA what you see on the other NMR, it is another substance, likely the 3,4-dimethoxymethamphetamine he suggested.

pastor - 25-1-2020 at 15:59

Sigmatropic: that's a really big peak for a residual solvent signal.

What I can say is that those two NMRs show different compounds :p

EDIT: the following analysis should have the warning that reading NMR is not exactly my strong suit

If I were to guess, the peak at 4.9 is the benzodioxole O-CH2-O shift. A carbon alpha to an ether increases the chemical shift from 1 to 3 ppm so at an acetal you might see something around 5 ppm. It's pretty rare for any moiety to have a peak here -- the only other thing is an alkene, which shouldn't be present. The high peaks are the aryl hydrogens.

Moving forward with this theory, the absence of the 4.9 peak in the second sample indicates that the "mehDMA" does not have a benzodioxole ring. Based on the descriptions of effects and the ability to simulate MDMA on test kits I suggest that the mystery compound is something like 3,4-dimethoxymethamphetamine. The "extra" peak around 3.7 is consistent with a phenolic ether, methinks.

Possibly, compounds like this are being introduced into the ecstasy supply by high-volume drug traffickers because they are cheap to produce and known to fool colorimetry.

[Edited on 25-1-2020 by clearly_not_atara]

Possibly, compounds like this are being introduced into the ecstasy supply by high-volume drug traffickers because they are cheap to produce and known to fool colorimetry.

Check the 3rd MDMAnmr sample.

This was MADE from safrole, and was NOT CUT... this sample is what started this whole NMR/MDMA debate XD. This was non darknet, private supplier type situation so it's def synthesis issue at least with a few/majority of the batches. We had the 3rd NMR looked at Bluelight and for all purposes it LOOKS like MDMA... so like meh i give up until we get more data

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

pastor - 25-1-2020 at 17:04

The magic sample looks just like the reference NMR plot from this paper: https://academicworks.cuny.edu/cgi/viewcontent.cgi?article=1... However, they mention something about 4.5 - 4.7ppm being a peak from the water used in the sample prep. So should that be ignored? How come it isn't in the other two plots?

pastor - 25-1-2020 at 17:07

What atara says has hand and feet.
It is not MDMA what you see on the other NMR, it is another substance, likely the 3,4-dimethoxymethamphetamine he suggested.

Aye even the nmr tester said that.. but look at NMR #3 MDMAnmr... that was the FIRST NMR that started this whole thing and is closer to MDMA

We had magic sample, sample A and sample B...

Sample A was MDP2-pol and MDMA but we can't find the NMR and we cant sample it anymore. We are trying to find it thou...

At this point we need a lot more Meh and magic samples

clearly_not_atara - 25-1-2020 at 17:30

Hm, no, the BDO peak is at 5.97. That makes water contamination more likely to explain the 4.87.

See:

http://www.scielo.br/scielo.php?pid=S0103-50532018000901944&...

But both of the "wrong" batches still have a large unexplained peak around 3.5-3.7. The "good" batch has only small peaks in this region. In the batch you claim was synthesized by a trustworthy lab this peak is at 3.489 and in the other bad batch it's 3.696.

pastor - 25-1-2020 at 17:32

Hm, no, the BDO peak is at 5.97. That makes water contamination more likely to explain the 4.87.

See:

http://www.scielo.br/scielo.php?pid=S0103-50532018000901944&...

But both of the "wrong" batches still have a large unexplained peak around 3.5-3.7. The "good" batch has only small peaks in this region. In the batch you claim was synthesized by a trustworthy lab this peak is at 3.489 and in the other bad batch it's 3.696.

Correct both of the "wrong" batches still have a large unexplained peak around 3.5-3.7 is about all we got so far. We are hoping for more info soon. But without more batches of meh and magic it is hard to go on. Sadly my exp is MDMA synthesis not NMR sadly. I only know someone with access to an NMR which has helped immensely

[Edited on 26-1-2020 by pastor]

clearly_not_atara - 25-1-2020 at 18:04

Unfortunately just about every fg potentially has a peak there

If I didn't know better I'd say it was free radical oxidation creating an -OH somewhere... but the likely products either a: are active (the N and the methyl), b: give radically different GCMS (anywhere on the propane/ring) or c: give radically different NMR (the methylene).

Another possibility is that the MDMA contains some proportion of 3,4-methylenedioxy-2-propanol. This would result from a failed synthesis, but again I'd be surprised it didn't come up on a GC/MS... it might be colorimetrically invisible since it's largely non-nucleophilic

pastor - 25-1-2020 at 18:19

Unfortunately just about every fg potentially has a peak there

We did have one batch of POL (tested via drugs data and came back 1:5 I think? ) and we tested it via nmr but We can't find that report sadly.

pastor - 25-1-2020 at 18:44

Unfortunately just about every fg potentially has a peak there

I know the trustworthy lab route was safrole, MDP2P via MEOH BENZ wacker... AL/HG. But no pol was detected via GC/MS when we did it... batch MDMAnmr. WHATever "it" is has the same mol weight of MDMA and passes reagents MMMS

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

j_sum1 - 25-1-2020 at 21:14

I'm going to go out on a limb here and say that this is a pretty fruitless endeavour of yours, pastor.

If you claim to be about harm reduction, you now have ample evidence that there is no quality control and there could be any amount of unidentifiable junk in what passes for an ecstasy tab. You can now make a pretty good case that people are shelling out cash for unknown swill and it is just as likely to be hazardous as it is to be ineffective.

You seem to overlook the fact that MDMA and its chemical cousins are prohibited substances in pretty much every country and with good reason. People die using this stuff. And countless more have their lives ruined by it.

It would be a better policy to steer people away from this stuff than to make such haphazard and unsystematic efforts in identification of random crap.

pastor - 25-1-2020 at 23:41

Quote: Originally posted by j_sum1

I'm going to go out on a limb here and say that this is a pretty fruitless endeavour of yours, pastor.

If you claim to be about harm reduction, you now have ample evidence that there is no quality control and there could be any amount of unidentifiable junk in what passes for an ecstasy tab. You can now make a pretty good case that people are shelling out cash for unknown swill and it is just as likely to be hazardous as it is to be ineffective.

You seem to overlook the fact that MDMA and its chemical cousins are prohibited substances in pretty much every country and with good reason. People die using this stuff. And countless more have their lives ruined by it.

It would be a better policy to steer people away from this stuff than to make such haphazard and unsystematic efforts in identification of random crap.

Well these tests are DETECTING differences. Much more so then GC/MS. ANd deter people. You know these people are. My CrYsTaL TuRnS StRiAgHT To BlAcK aNd EC Says 97%... Good luck telling those people. Even getting people to admit ALL MDMA on CG/MS is not equal is like pulling hairs getting ANYONE to believe us, hence the post here. Getting people to admit we have a difference between most old market vs new market MDMA, cuz us old times did too much MDMA... RIGHT..

We believe it is possibly caused by a lack a methylamine and or failure to distill the freebase before gassing. We will need more samples, which we are procuring and we do have someone reading the NMR in depth. At this point it's all data driven and we need more data!!! But we are finding patterns

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

stoichiometric_steve - 26-1-2020 at 04:26

At this point it's all data driven and we need more data!!! But we are finding patterns

At this point i think you grossly overestimate everybody else's interest in figuring this out.

Why don't you just make sure you start with clean and proper materials instead of trying to crowdsource knowledge about what went wrong with your cooking? There is no mystery to this: Either you put in shit or you done shit. Solved.

Established synthetic pathways reproducibly give correct products. Whatever went wrong with yours, who knows and who cares?

clearly_not_atara - 26-1-2020 at 07:45

I agree with SS that the title is invalid. There are plenty of people myself included who have had magical experiences on MDMA synthesized in this decade.

A better question might be “why do some batches of MDMA seem to be unusually weak?”. In this framing there is the potential for contamination by some inactive impurities such as MDP2Pol, N,N-dimethyl-MDA, occurring rarely.

Texium - 26-1-2020 at 08:00

I'd bet money that spectrum "...207" was run in methanol. The unlabeled peak at 3.31 corresponds to the solvent residual signal of methanol, and there is always a lot of water present in deuterated methanol if it's been opened before. That big 4.87 peak is exactly where water shows up in methanol. If D₂O was the solvent it would be seen around 4.79. So there's nothing amiss with that sample, it is reasonably pure.

The other one does look like it was done in D₂O (presumably as the HCl salt) albeit maybe not properly referenced. I'm not sure why the multiplet around 3.3 is not integrated. That should correspond to the proton on the tertiary carbon. If you consider that, then there must be some spurious junk in the peak around 2.5 that is integrated as 5 (should come out to 4), plus there's that quartet at 3.38. A quartet often implies an ethyl group.

I'm not too familiar with potential impurities that may be present, so I won't go out on a limb to guess at what could be in there, especially since it's hard to see what exactly is going on in that 2.5 peak. Having the original raw data to look at more closely in Topspin would be nice. Barring that all I can say is that your "meh" stuff does indeed look "meh."

pastor - 26-1-2020 at 09:09

Quote: Originally posted by stoichiometric_steve

At this point it's all data driven and we need more data!!! But we are finding patterns

BECAUSE, my lab is one thing... That can easily be fixed, we can reun with excess of methylamine, ran a DMF wacker vs MEOH, etc, etc ... BUT MOST MDMA IS DARKNET DUTCH DIRT... they are having the same issue. Tests at 97% MDMA but doesn't get you quite high, needs 200+mg to feel ANYTHING and even then they don't smack unlike the 80-120mg of yesteryear. We aren't trying to fix my batch. We are trying to fix the WORLD MARKETS OF MDMA.

Hopefully someone in the clandestine scene will listen to us when we do find the issue, but this isn't about fixing "our product" That is as simple as rerunning our batch or doing a different animation... No we are trying to fix the world's supply for the most part. Why are SO MANY labs are creating meh and where/why did all the magic go. Hence the large effort on bluelight, why we want to find out the issue, the impurity/s and how we can clean it and turn meh into active magic. Either by means of middle men cleaning bulk product via column or recrystallization. We want to find out the most common causes/issues so we can clean product, and why so many dutch superlabs seem to be making meh.

My guess is PROBABLY happening during animation but that is all I have to go on.

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

dextro88 - 26-1-2020 at 09:58

The only difference between the old stuf you are speaking of and the nowadays is the precursor the MDP2P is derrived, but i cant find what that a big difference can make, have had some stuff that isnt produced from glycidate and it rocks have had some stuff that is from the DNM and i just consider it cutet as a higher dosage was needed for the same results but i dont get your problem MDMA still is almost number 1 choise of drug users who want to rave, so shurely the magic is still there...

[Edited on 26-1-2020 by dextro88]

pastor - 26-1-2020 at 10:37

Quote: Originally posted by dextro88

The only difference between the old stuf you are speaking of and the nowadays is the precursor the MDP2P is derrived, but i cant find what that a big difference can make, have had some stuff that isnt produced from glycidate and it rocks have had some stuff that is from the DNM and i just consider it cutet as a higher dosage was needed for the same results but i dont get your problem MDMA still is almost number 1 choise of drug users who want to rave, so shurely the magic is still there...

[Edited on 26-1-2020 by dextro88]

Our private lab batch WAS SAFROLE and reductive animation was Al/Hg. SO it is not Glycidate vs safrole debate that flew out the window with NMR analysis #1... And yes, I have a batch of MAGIC from a burning man source not darknet so it's more "family" product. People on the hive in 1997-04 complained of inactive/meh product as well from safrole, it just wasn't as common. If you read the all the bluelight pages you'll find a few reports

You are missing that Reductive amination process also changed from lukehart and Al/Hg to catalytic hydrogenation via platinum, adams catalyst or H2 for yield/purity... Borohydrides are slow for clandestine on the dutch scale. While i'm sure the lukehart MDA/MDMA had something to do with SOME of the old magic... It is def not indicative of the magic that floats around now. Also I see a LOT more MEH than magic and it's fooling Energy control Darknet avengers MDMA testing. That is for sure.

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

clearly_not_atara - 26-1-2020 at 10:53

So here's my rationale for MDP2Pol and/or N,N-dimethyl-MDA (MDDM) appearing as synthetic impurities in MDMA synthesized by reductive amination of MDP2P with MeNO2 under acidic conditions:

- direct reduction of the ketone leads to MDP2Pol, this should be unlikely but may occur with excessively high temps / too much reducing agent

- the Nef reaction on MeNO2 generates formaldehyde, which may reductively aminate MDMA to MDDM.

But neither possibility acceptably explains the 3.5-3.7 peak.

There is another peak that changes in the good sample relative to the "meh" samples, around 2.7. The "meh" samples have peaks around 2.55-2.59 but the good one is at 2.71. This shift is small but it could be meaningful. Published NMR spectra of MDMA tell me that this peak is typically located on the N-methyl group and furthermore that it should be at 2.7, which does suggest that we're getting somewhere.

In fact, since the NH proton apparently does not appear in the NMR spectrum (can someone confirm?), I think this shift could be consistent with double N-methylation leading to MDDM impurities.

Reference NMR attached.

pastor - 26-1-2020 at 11:15

So here's my rationale for MDP2Pol and/or N,N-dimethyl-MDA (MDDM) appearing as synthetic impurities in MDMA synthesized by reductive amination of MDP2P with MeNO2 under acidic conditions:

- direct reduction of the ketone leads to MDP2Pol, this should be unlikely but may occur with excessively high temps / too much reducing agent

- the Nef reaction on MeNO2 generates formaldehyde, which may reductively aminate MDMA to MDDM.

But neither possibility acceptably explains the 3.5-3.7 peak.

There is another peak that changes in the good sample relative to the "meh" samples, around 2.7. The "meh" samples have peaks around 2.55-2.59 but the good one is at 2.71. This shift is small but it could be meaningful. Published NMR spectra of MDMA tell me that this peak is typically located on the N-methyl group and furthermore that it should be at 2.7, which does suggest that we're getting somewhere.

In fact, since the NH proton apparently does not appear in the NMR spectrum (can someone confirm?), I think this shift could be consistent with double N-methylation leading to MDDM impurities.

Reference NMR attached.

He made and purified the methylamine from I believe hexamine and did not use nitromethane. Nitromethane was not used at all. AT least this is what I know from our private lab MDMAnmr batch made from safrole. I think he did say his mantle has having temp swings, which could also make sense of MDDM...

I do not know if you are implying about meh batch 1 or 2... If it helps MDMAnmr #1 a uvspot test was done yesterday. Shows there is only 1 compound. It showed there was an amine and there are no other amines active or not. He stained the TLC with ninhydrin. I can upload the plates UV and non UV later if you want

PS thank you for everyone who has taken the time to lookover our NMR reports and while some people think we are crazy, there is something happening on a scale that we would like to figure out

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

KEWL

sodium_stearate - 26-1-2020 at 11:32

This is turning into a KEWL place!

Great. Go to burning man. Get stoned out of your mind
and fry some brain cells.

If that aint KEWL, I don't know what is!

pastor - 26-1-2020 at 11:53

Quote: Originally posted by sodium_stearate

This is turning into a KEWL place!

Great. Go to burning man. Get stoned out of your mind
and fry some brain cells.

If that aint KEWL, I don't know what is!

Some people don't DO drugs but find MDMA synthesis interesting, some people find lab analysis interesting, some people only sell drugs and want to have quality product for their clients. Regardless we had someone look at NMR analysis #1 and he said on the surface the MDMA appears to be MDMA . If you don't find it interesting or COOL or interesting that GC/MS is being fooled and fooling Energy control, Drugs data and private labs (friend who has access to NMR) Then this conversation isn't for you.

If you do find it interesting that GC/MS , MALDI, UltraViolet–Visible Spectroscopy and other tests are being fooled then please join the conversation in a positive manner

We are not discussing MDMA synthesis which is against forums rules, but why and how reliable are these tests in the first place. At least 1 or 2 people find it interesting and are willing to contribute in a positive manner or light for one reason or another.

[Edited on 26-1-2020 by pastor]

clearly_not_atara - 26-1-2020 at 12:19

Quote:

How do you know this? How can you respond so quickly about a synthesis that someone else carried out years ago?

Quote:

If it helps MDMAnmr #1 a uvspot test was done yesterday. Shows there is only 1 compound. It showed there was an amine and there are no other amines active or not. He stained the TLC with ninhydrin. I can upload the plates UV and non UV later if you want

Ninhydrin does not react with MDDM or other tertiary amines

Quote:

BUT MOST MDMA IS DARKNET DUTCH DIRT... they are having the same issue. Tests at 97% MDMA but doesn't get you quite high

This is simply false. Again, it contradicts the experiences of thousands of people who get high just fine

[Edited on 26-1-2020 by clearly_not_atara]

stoichiometric_steve - 26-1-2020 at 12:21

We aren't trying to fix my batch. We are trying to fix the WORLD MARKETS OF MDMA.

…

We want to find out the most common causes/issues so we can clean product, and why so many dutch superlabs seem to be making meh.

Why would ANYONE here help out ORGANIZED CRIME who apparently "don't know how to cook their shit"?

Do you know what's really wrong with them? They cook whatever shit it takes to make money, not to give you magical experiences. Nobody gives a shit about you or your drug buddies or your trips. For all they care, after you give them all your money, you can die in a ditch.

The only thing you can and should do is rally for controlled legalization.

clearly_not_atara - 26-1-2020 at 12:22

Quote: Originally posted by stoichiometric_steve

Why would ANYONE here help out ORGANIZED CRIME who apparently "don't know how to cook their shit"?

Look man I don't know if this is still a chemistry forum but I find the NMR discrepancies interesting. We have three batches, one good, two bad, and some correlations.

pastor - 26-1-2020 at 12:43

Quote:

How do you know this? How can you respond so quickly about a synthesis that someone else carried out years ago?

Quote:

Ninhydrin does not react with MDDM or other tertiary amines

Quote:

BUT MOST MDMA IS DARKNET DUTCH DIRT... they are having the same issue. Tests at 97% MDMA but doesn't get you quite high

This is simply false. Again, it contradicts the experiences of thousands of people who get high just fine

[Edited on 26-1-2020 by clearly_not_atara]

Ah good question, you see the batch was made Oct 28th of 2019, arrived halloween day with me and a DRUG virgin who has only done small amounts of cocaine. She did not roll until after 250+ to 350mg. The product was then tested nov. 18th via NMR via another friend after he ran GC/MS and MALDI came up positive for MDMA thou he SWORE up and down 97% via GC/MS and MALDI confirmation. I asked did you get high he was like no not really, then thus then he ran a NMR

I know the route because I was in contact with the person as The source of safrole was provided by me, it is still QUITE COMMON in 2019/2020 in the USA if one looks hard enough... my results via analysis show it is still QUITE available without any regulation if you look the correct way. (no i'm not gonna tell anyone go away) and @stoichiometric_steve I only gave him a VERY small amount of safrole... like 2 to 3 oz yeez. Some kingpin you make me out to be

Anyways he also detailed the route via messages and I could go back anytime, thou it would be a huge pain the way we kept in contact. Hence why/how I know so much and can respond so quick it's only been 2.5 months . And he made it from Formaldehyde + Ammonium Chloride not hexamine my bad close enough thou to exclude nitroethane. He followed brightstar according to my records but made his own p-Benzoquinone from hydroquinone . I even remember the picture of p-Benzoquinone he made. The product was acetone washed 2-3 times, but was not recrystallized.

Also while magic is still around (I have recently bought some, If you search bluelight everyone is asking which darknet dealer has magic and no one seems to have an answer but that's just what I know) My last 3-4 dealings on the darknet have been MEH and I haven't got magic online in ages but I haven't bought online since like 2017/18. Maybe i'm wrong, magic does exist but even my own supplier has issues finding someone with good stuff.

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Yeah, extremely rare, if not impossible, to find MDMA that looks like that on the DN. I’ve been buying exclusively from markets for the past 3 years and have never come across any.

Others may have had better luck than me though. see thread

https://www.bluelight.org/xf/threads/what-is-wrong-with-the-...

There are variations of the MEH stuff some active at 200-250mg, But your not rolling , it doesn't come in "waves" , you need at least 200 mg to feel something, Your pupils are not saucers, You do not sweat super easy.Yes you can feel the meh stuff and it canget you high, of course but oldtimers can tell a difference, from time to time a batch of magic does come thru but from my experience most darknet MDMA is meh, along with people's exp on bluelight. Does magic active stuff exist yes, have I found it, yes but I think for every 1 good batch is around 5 bad batches (norcal molly scene most people at least reagent test here) , a good example is when I look at my local rave scene. People on this "new stuff" zone out and are zombies/lethargic. They lack any energy. This is from my exp at local renegades where it's a more family scene, I avoid big shows and only go to the hippy music festivals. I'm not sure what your guys exp with MDMA is but enough reports are coming in that SOMETHING is causing a huge issue and people taking 300-500mg in a night is a HUGE nono. I use to think MDMA is MDMA, A result Frpm energy Control of MDMA is MDMA then I got this meh batch and my view 100% changed. NMR's seem to confirm that and Maldi and GC/MS is not accurate it appears. We can't explain what MEH feel like only that people new to MDMA think it's MDMA but something is off/dulled. It will get people high just 200mg doesnt make you roll tits like 80-120mg of magic will that's all I have to say about that in mine and others experiences of the current markets in our area.

[Edited on 27-1-2020 by pastor]

Dain Bramage

sodium_stearate - 26-1-2020 at 13:50

What would happen if these samples were tested
by an independent lab, by qualified research chemists
that are not users of the substance being tested?

My theory is that they'd find the answer.

pastor - 26-1-2020 at 14:00

Quote: Originally posted by sodium_stearate

What would happen if these samples were tested
by an independent lab, by qualified research chemists
that are not users of the substance being tested?

My theory is that they'd find the answer.

Sadly almost noone has access to an NMR, and to be fair he has only sampled 1 of the 3 NMR samples that was meh sample 1. Reading NMR is not his strong suit he just works in a lab with access to one. We have someone else attempting to reading them on bluelight but he has been busy and wants to read the report correctly. We did post here to get more people involved thou as to speculate what is wrong. AT least 1 person finds it interesting so I give it that.

I remember about oh 4-5 years I remember a darknet vendor called caslava, he had a $10k bitcoin bounty on his xanax to disprove his 99.X % pharma purity. I wish I had access to NMR back then lmao. I only met someone last year with one. And trust me I ASKED.... WHen asked why he wouldn't take an energy control GC/MS he said it was garbage. These MDMA samples pretty much confirm our suspicion about that. Also I sent xanax powder that looked like crushed pills and had no bitter xanax taste, Energy control said 99% xanax even thou clearly not true. Hence My understading of Caslava hating GC/MS

[Edited on 26-1-2020 by pastor]

[Edited on 26-1-2020 by pastor]

G-Coupled - 26-1-2020 at 15:00

Was the crushed powder active at all when ingested? I wonder what it could've been?

Are all GC/MS analyses created equal? I don't mean screwing up the procedure (although I'm sure that happens plenty), more like do all the devices produce pretty much the same data given a particular sample?

Are the different models of GC/MS significantly different from one another? Do we know which machines Energy Control might be using?

[Edited on 26-1-2020 by G-Coupled]

pastor - 26-1-2020 at 16:49

Quote: Originally posted by G-Coupled

Was the crushed powder active at all when ingested? I wonder what it could've been?

Are all GC/MS analyses created equal? I don't mean screwing up the procedure (although I'm sure that happens plenty), more like do all the devices produce pretty much the same data given a particular sample?

Are the different models of GC/MS significantly different from one another? Do we know which machines Energy Control might be using?

[Edited on 26-1-2020 by G-Coupled]

My meh MDMA was active but in the 200-300 mg sadly. I have no idea if all GC/MS is equal BUT it seems most if not all labs have been missing something with GC/MS probably peaks overlapping. Sadly my knowledge is is routes not analytics

[Edited on 27-1-2020 by pastor]

pastor - 26-1-2020 at 17:34

Updated Meh batch1 NMR.

The product was ran thru a silica column and is now more in line with product magic. I have no idea the yield/loss. This was the TLC uv product I talked about earlier.

Attachment: 20200126202140202.pdf (135kB)
This file has been downloaded 414 times

Texium - 27-1-2020 at 11:01

Yep, that looks like reasonably pure MDMA. Surprise, surprise: apparently subjecting an impure product to a purification procedure yields a purer product.

SWIM - 27-1-2020 at 11:30

Quote: Originally posted by Texium (zts16)

Yep, that looks like reasonably pure MDMA. Surprise, surprise: apparently subjecting an impure product to a purification procedure yields a purer product.

You will not laugh!
You will not cry!
You will purify your products!

This is my chromatography column
There are many like it, but this one is mine.
It is my life.
I must master it, as I must master my life.
Without me, my column is useless.
Without my column, I am useless.

This is my column, this is my gun.
This is for purification, this is for fun.

ermy chromotography.jpg - 6kB

karlos³ - 27-1-2020 at 12:21

So you guys use improperly purified product and then wonder why it is not acting as expected?
What can I say except, this is a cookery attitude, not chemistry.

pastor - 27-1-2020 at 12:32

So you guys use improperly purified product and then wonder why it is not acting as expected?
What can I say except, this is a cookery attitude, not chemistry.

Considering how 90%ish of the market is impure shit... It is much more then just my product... WHich is the cookery attitude of the majority of the markets. It seems even thou our product was QUITE pure from the NMR guy testing it... We are talking about something that maybe mg active prevent the reaction/bioavailability of MDMA. Multiple acetone washes were done before the product was handed to me originally.

WE are sending the fraction to NMR but we aren't sure if we will find anything interesting. AT least this is what NMR guy thinks. Possibly a metal who knows

[Edited on 27-1-2020 by pastor]

karlos³ - 27-1-2020 at 12:44

But you're among chemists here, we don't use such crappy products with only 90%.
Was it even vacuum distilled, it sounds like it wasn't?

karlos³ - 27-1-2020 at 13:30

Acetone washed, wow, it was not even recrystallised?
Do you know how recrystallised MDMA has to look like?
I attached a picture.

Tsjerk - 27-1-2020 at 14:10

Just washed with acetone... Yes, so you got rid of everything that is not an amine. Congratulations.

What would be interesting is getting an GCMS or NMR, or both on the fractions that aren't MDMA. Why don't you do this? You did a column chromatography right?

pastor - 27-1-2020 at 16:04

Quote: Originally posted by Tsjerk

Just washed with acetone... Yes, so you got rid of everything that is not an amine. Congratulations.

What would be interesting is getting an GCMS or NMR, or both on the fractions that aren't MDMA. Why don't you do this? You did a column chromatography right?

We are doing this right now don't worry

SWIM - 27-1-2020 at 16:16

Using NMR to find out what's wrong with a product you didn't re-crystallize is like using a CAT scan to find out why hitting your TV really hard didn't fix it.

pastor - 27-1-2020 at 16:37

Quote: Originally posted by SWIM

Using NMR to find out what's wrong with a product you didn't re-crystallize is like using a CAT scan to find out why hitting your TV really hard didn't fix it.

To be fair we believe this is the common issue with mass produced MDMA. But we didn't realize such small impurities could have such drastic effects, even the guy running the NMR is unsure if we will detect anything but he will give it a shot when he has time.

[Edited on 28-1-2020 by pastor]

Tsjerk - 27-1-2020 at 23:04

Quote: Originally posted by SWIM

Using NMR to find out what's wrong with a product you didn't re-crystallize is like using a CAT scan to find out why hitting your TV really hard didn't fix it.

If you have done your column chromatography correctly you can characterize any impurity. Just concentrate the fractions you expect your impurity to be in. You only need a couple milligrams for either NMR or GCMS. I would go for GCMS..

If you can't you have to redesign your column chromatography. Longer column, different solvents, more gradual slope of concentrations...

NMR is nice, really nice, but only to see if something is there or not. If you don't see a peak? No, it is not there. If you do see a peak? Yes, those atoms are there! But when you are getting peaks you can't explain? Then you have to go to GCMS for example.

woelen - 28-1-2020 at 03:42

It is time to add something new and interesting in this thread and to increase its level. Keep in mind that this is a thread on material upon which many people frown. So, only if you really have to add something interesting from a chemical point of view, add this. Complaining about meh quality of MDMA does not add anything new.

Up to now I have not seen much more than the shocking conclusion that purification of a product leads to a purer product.

Maybe that is the maximum level people can attain when using MDMA ???

[Edited on 28-1-20 by woelen]

XeonTheMGPony - 28-1-2020 at 03:49

So you guys use improperly purified product and then wonder why it is not acting as expected?
What can I say except, this is a cookery attitude, not chemistry.

all of this seems half assed cookery, right down to the language.

Garbage in garbage out, and frankly even taking an aspirin carries risk.

Simple if you want to enjoy life don't fuck with your bodies chemical systems by dumping crap in it that will screw with the natural balance unless demonstrable need is shown. Poof Harm has now been reduced!

[Edited on 28-1-2020 by XeonTheMGPony]

stoichiometric_steve - 28-1-2020 at 04:31

Quote: Originally posted by XeonTheMGPony

So you guys use improperly purified product and then wonder why it is not acting as expected?
What can I say except, this is a cookery attitude, not chemistry.

all of this seems half assed cookery, right down to the language.

Just what i've been saying all along. This isn't about some heroic mission, this is about finding out why your product sucks and — suprise! —it's because you're a shitty chemist.

j_sum1 - 28-1-2020 at 04:49

Quote: Originally posted by XeonTheMGPony