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What is wrong with the MDMA available today?

indigoaura

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Jan 4, 2009
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Apologies if this was already discussed before, but do these compounds not easily filter out with say, an acetone wash?
Not based on what we have observed, no. Quite a few people have tried acetone washes as well as re-crystallization. From my understanding, column chromatography is what needs to occur to separate them.
 

user666

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Feb 13, 2020
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Also, I am excited that heart rate (BPM) appears to be a variable that we can track easily according to the chart on page 9. It seems that the difference should be especially notable around the 1.5 hour mark. What do you think @user666 ? A lot of people have an I-Watch, Fitbit, or something similar that could track this.
Yes, besides Epinephrine, the confidence of these physiological indicators was very high in this study (p<0.001). All of them except Epinephrine, more than doubled when under influence of MDMA only. However the baselines of these physiological indicators are very individual so they would only be reliable if the same individual logged his HR (BPM), SBP, DBP with Meh MDMA and some time later with known Magic MDMA.
A baseline readings when not dosed with anything and in the same controlled environment (not excited), would be useful, too.



The blood Glucose level belongs to a different class of indicators because its increase is a very unusual event while fasting. This is in contrast to HR (BPM), SBP, DBP, MAP which can increase for many other reasons.

Anyway, it seems we are back to the same problem: acquiring MDMA-naive subjects and both kinds of MDMA.


SBP = Systolic Blood Pressure, DBP = Diastolic Blood Pressure, MAP = Mean Arterial Pressure, HR = Heart Rate (expressed in Beats per Minute [BPM] )
 
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user666

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Feb 13, 2020
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Apologies if this was already discussed before, but do these compounds not easily filter out with say, an acetone wash?
It is not a matter of filtering - it is a matter of different solubility in different solvents. MDMA HCl is slightly soluble in anhydrous Acetone.
The polarity of these compounds is the same as MDMA so their solubility is the same. Tosylation has not been tried, but it has a theoretical potential to remove the HMCA.

Anyway, many people have tried Acetone washes. These that did it with hydrous Acetone lost a lot of product and those that did it with anhydrous Acetone reported only slight improvement, e.g. better color and smell of the product due to removal of other contaminants than the one we are after.
 
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indigoaura

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Anyway, it seems we are back to the same problem: acquiring MDMA-naive subjects and both kinds of MDMA.
I guess I am seeing it differently.

We are not researchers. We are not going to be the people to set up and orchestrate and publish a study about this.

While I see how having MDMA-naive subjects would be beneficial, I don't see that as a primary need right now.

I'm focused more on analyzing the product. I have batches of Meh, @G_Chem and others have batches of magic. If I could just find labs to work with to give us the info we need, that would be a great development.

Also beneficial, if we could develop some kind of "column chromatography for dummies" system that would allow most people to purify their product and separate impurities.

Worry about testing the theory on MDMA naive people later. If we could 1. confirm the presence of impurities, 2. figure out a way to remove those impurities, and 3. confirm that purified product regained the lost subjective effects, then we would be on very solid ground with this particular hypothesis.
 
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topgunner19

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Yep, great coke definitely went the way of the dinosaur. And very similar to todays MDMA story, coke of the 70's-90's was fully oxidized thus the high from it was what dreams were made out of. Todays coke, though it still tests positive for cocaine, is not oxidized and contains 10-12 other alkaloids that alter and ruin the true cocaine high.

As with todays MDMA, the production has resulted in changes due to the lack of safrole which means MDMA thru a different synthesis. As a result, I believe the theory of todays MDMA favoring the R isomer over the S isomer. The result is a lackluster end product, though still MDMA compound, the high is nothing close to S isomer favored MDMA.

And the Dallas Groups product was pure MDMA, made correctly I might add ;-)
Think you are correct on pre cursors
The soft white clumpy stuff so gentle lovey dovey vs shards or huge moonrocks glass like that seems to grt you on a more racey buzz trip vs a loved up
 

AutoTripper

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Feb 28, 2019
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What makes me chuckle, or slightly angered, unless I have gotten this wrong- years back, there was this big guilt trip thrown on wordwide MDMA users- Oh, the precious Saffrole population is approaching extinction.

Solution- chop them all down! (If that's what they actually did, I havent followed this scene like most of you to be clear on any facts.)
 

user666

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I guess I am seeing it differently.
You idea has merits.

Also beneficial, if we could develop some kind of "column chromatography for dummies" system that would allow most people to purify their product and separate impurities.
It would be difficult. Most people are not dilligent and precise enough and would not be able to handle chemicals such as pure solvents and silica gel even if you made a kit for them.
The compounds that are to be separated are transparent/invisible so they require stains (more chemicals to handle) or UV light to visualize them. Glass blocks UV so with this method quartz needs to be used to let UV through. Quartz is more expensive than glass.

3PCircle and you seem dilligent and intelligent enough to handle it but I do not know about about your eye-hand coordination needed to maintain precise packing, dripping and a coherent solvent front.
 
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Jmoda

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Jun 11, 2020
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Think you are correct on pre cursors
The soft white clumpy stuff so gentle lovey dovey vs shards or huge moonrocks glass like that seems to grt you on a more racey buzz trip vs a loved up

And what happens when you crush up white shards or milky moonrocks? They become soft white....i dont think powder vs rocks is really a differentiator.
 

ThreePointCircle

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Apr 21, 2016
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It would be difficult. Most people are not dilligent and precise enough and would not be able to handle chemicals such as pure solvents and silica gel even if you made a kit for them.
The compounds that are to be separated are transparent/invisible so they require stains (more chemicals to handle) or UV light to visualize them. Glass blocks UV so with this method quartz needs to be used to let UV through. Quartz is more expensive than glass.

3PCircle and you seem dilligent and intelligent enough to handle it but I do not know about about your eye-hand coordination needed to maintain precise packing, dripping and a coherent solvent front.
I had two goes with doing a column. First time round was a bit of a mess, but second was tidy and looked good from a method point of view. Problem was: a) what solvent system to use and b) how to work out what fractions had what

I think normally the fractions are tested with tlc. My most recent tlc experiments (a couple of months ago) had me switching to bigger plates. But they had massively different rf values from the other plates I was using. So it appeared to me that there's a huge solvent/stationary phase effect and I have no idea how that translates to running a column. Like how do you know you're going to get good separation?

I did try using reagents to see if anything was coming out but no luck really. I would be up for doing it again, definitely, but I just don't know how to get the solvent right and know what the output is.
 

indigoaura

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I had two goes with doing a column. First time round was a bit of a mess, but second was tidy and looked good from a method point of view. Problem was: a) what solvent system to use and b) how to work out what fractions had what

I think normally the fractions are tested with tlc. My most recent tlc experiments (a couple of months ago) had me switching to bigger plates. But they had massively different rf values from the other plates I was using. So it appeared to me that there's a huge solvent/stationary phase effect and I have no idea how that translates to running a column. Like how do you know you're going to get good separation?

I did try using reagents to see if anything was coming out but no luck really. I would be up for doing it again, definitely, but I just don't know how to get the solvent right and know what the output is.
The solvent issue is the big unanswered question for me as well. I would be willing to invest the capitol to make column chromatography happen, but if I am using the wrong solvent, it is not going to be worth the investment.

I was just reviewing your experiments on the Wiki, @ThreePointCircle. Your experiments show the separation of two compounds. I just don't know how to proceed from there. Did you ever reach out to Wedinos about analyzing the plate? Drugs Data never replied to me about that.
 

user666

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Feb 13, 2020
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229
I think normally the fractions are tested with tlc. My most recent tlc experiments (a couple of months ago) had me switching to bigger plates. But they had massively different rf values from the other plates I was using. So it appeared to me that there's a huge solvent/stationary phase effect and I have no idea how that translates to running a column. Like how do you know you're going to get good separation?
Obviously the silica on the TLC plates has to be similar to the one in the column.
The rest is explained in this video.
 

Biscuit

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Dec 27, 1999
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Good grief finally some sanity.

Thank you indigo for resurrecting the article regarding the inhibiting dimer impurities, which if in enough concentrations could very well turn a magic experience into meh.

Anyway this article is essential reading so I’m reposting the link - https://zero.sci-hub.tw/2640/a20cf55121d0f8686e4c6ab1cdb88b65/pifl2005.pdf

I tried to post about this a few weeks ago but it went nowhere and my hypothesis relating to this issue was lost in the wash as no one could remember where the article was in the 280 pages etc.

At the outset, this article refers to the two dimers 12 and 13 being produced from the Leuckhart reaction, however, the article is also from 2005 and long before PMK glycidate and our problem came along. The other thing to note is that dimers of this nature would come in a large number of different molecular variations depending on the manufacturing steps and reagents used and for all we know similar but far more potent inhibitory compounds might result if modern day reagents are used.

I have reposted my post about this below but in short, forget about the Leuckhart, because I think you’ll find that since 2012 this article may have far more relevance to MDMA production that extends well beyond the Leuckhart. Further, the “limiting reagent in the reductive amination” crap I was banging on about is actually irrelevant as the critical diarylacetone molecule is actually created earlier; this being the part I couldn’t remember without the article. (I do completely understand why I was challenged on that aspect of what said, which regardless of who is right, doesn’t effect the point below.)

ANYWAY....

Have a look at Figure 2 at top of page 348, which starts with the MD equivalent of phenylacetic acid, which when reacted with acetic anhydride in sodium acetate produces MD-P2P but this side reaction occurs, where two molecules get stuck together and we effectively have a PMK dimer. This molecule then produces 12 and 13 if put through a Leuckhart amination, although a normal reductive amination should still produce something similar at the end of the day.

Well what happens with PMK glycidate and it’s various incarnations when it is hydrolysed in an attempt to get PMK? What’s produced? What else is produced? What factors might favour the production of certain molecules as opposed to others. Does anyone actually even know? Where are the reaction mechanism diagrams for this method, coz I haven’t found any?!

Well some clever person should spend some time on it because the sort of products you might get as well as PMK are MD-phenyl acetic acid, acetate ions and maybe even something approaching the reactive part of an acetic anhydride molecule. Which all adds up to potentially large amounts of diarylacetone byproducts being made with the PMK and which sloppy technique wouldn’t remove or bother with.

Throw in the talk of this one pot reductive amination with either methylamine or nitromethane and one might end up with all sorts of molecules looking an awful lot like 12 and 13 if not those same ones as well. And because PMK glycidate comes in several forms, this could increase the extent (in both quantity and variety) to which this might occur; from batch to batch, and from one level of Meh factor to an even greater level of Meh factor if you will.

PMK from safrole and which was then turned to MDMA via a non Leuckart reduction would not have this problem. I honestly believe PMK from the glycidate especially without care and purification might produce these sorts of compounds as good as any route the scientists have commented on.

These compounds could be detected by government Laboratories if they were looking for them but they would only do that in a particular case to match batches with other batches. However, researchers of this calibre could certainly analyze samples and provide this level of detail if asked and no doubt paid for.

I Really believe this or something close to it must be the answer and I invite anyone to tell me I’m talking nonsense and why that is so.

www.bluelight.org/xf/threads/what-is-wrong-with-the-mdma-available-today.791073/post-14929097

Aug 21, 2020
There is no doubt in my mind there is a difference. (You nailed it HerpDerpMcDerp; and welcome to Bluelight.)

I’ve been taking MDMA pills and MDMA powder/crystal for 21 years now and after almost giving up, two months ago I had my night rocked by a 120mg dose of the most luscious, munty (of the more cheeky/naughty kind), and long lasting (with God forbid actual afterglow), MDMA crystal in many years. I was on night two as well, having used meth all day prior. Had I been younger, on night #1 and just generally less trashed, this stuff would have been the magic that I remembered from years ago, magic that I have barely encountered in Australia for more than ten years.

After earlier championing the SvsR isomer issue, I am now positive the answer to this entire issue is contained in the article indigoaura posted many pages ago, where very small quantities of two structurally similar dimers created as impurities during MDMA manufacture, could cause significant inhibition of the MDMA effects at comparatively very low amounts by binding to the neurotransmitter reuptake transporters, much like how for prescription SSRIs and SNRIs nullify the effects of MDMA into something resembling “Meh” in those people taking these drugs. (Didn’t one of the dimers show ridiculously strong affinity to ALL THREE of the significant transporters, the noradrenaline, the dopamine AND the serotonin?! A higher presence of such a chemical in a substance purporting to be “pure MDMA” is going to completely fuck up the roll and will need a much greater dose to get anywhere close to something resembling a roll.)

Whilst I would like to put together a much more thought out, well researched and diagrammatically useful post, as I have been false starting on this endeavour for months now, I thought it better to put something out there for discussion without any further delay.

It is clear that PMK glycidate could favour the creation of these dimers, especially if the PMK is not properly purified. I mean what is created when the glycidate molecule is hydrolysed, acetic acid or acetate perhaps, the very reactant which they list in one of the initial steps that gives rise to these dimers.

The other matter of significance is that of what the limiting reagent is in the reductive animation step of PMK and methylamine Into MDMA. This reaction always ideally proceeds with a significant excess of methylamine to PMK, for if there is no excess, the formation of these dimers or molecules like them is much more likely to occur.

In the old days, as it was safrole/isosafrole and the PMK produced from these that was in the shortest supply, there would never have been any question about having an excess of methylamine to this highly sought after and almost impossible to obtain precursor. However, we know now that PMK glycidates are widely available in massive quantities and so PMK is no longer going to be the limiting reagent in the reductive amination. Instead, not only might manufacturers fail to properly purify the PMK or otherwise proceed via one-pot synth straight to MDMA with potentially highly reactive hydrolysis products from the glycidate (with certain PMK glycidates being worse than others for creating such dimers, this being a further reading for different levels of “meh”), but they may be skimping on the methylamine in the reaction as well, such that there is now an undue excess of PMK made from glycidate relative to the methylamine, a factor which would strongly favour the creation of these inhibiting dimers to a much greater degree. Throw in the fact that platinum catalyst hydrogenation is now almost always used to reduce the imine as opposed to borohydride, and it’s anyone’s guess as to what mess we actually end up with.

The above hypothesis would account for why there are varying degrees of Meh (being the extent to which the MDMA does or does not have the presence of such impurities, a fact which the right laboratory could actually
test for), why safrole produced MDMA doesn’t create this problem to the same degree, and why the change to the almost infinitely available glycidate pre-precursor may have skewed the reaction in the wrong direction on account of commercial considerations (despite the news now of stupidly high dosages of this crappy
MDMA).

As an aside, for a long time high purity racemic methamphetamine produced from p2p has received similarly poor user reports along the lines mehMDMA despite being >90% purity - “mehMeth” if you will. And where is this P2P coming from but BMK glycidates, the PMK glycidate equivalents. Precisely the same reaction considerations to what I have described above for MDMA would apply for methamphetamine produced via this route and where the more readily available precursor might also be present in relative excess to the methylamine needed
for the reductive amination. If similar dimers
were produced (and I’ll find an article I have saved confirming this very thing), then these too would likely inhibit the action of the meth in similar ways.

Sorry that this post is so garbled but the earlier discussion about this and articles i refer to are buried somewhere a hundred pages or so ago. As this thought has otherwise been bubbling uselessly away in my mind for more than six months now, best I just get it down and hope that the more cleverer chemists and those more familiar with the invaluable content in these almost 300 pages, could give it further consideration
 
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user666

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Feb 13, 2020
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Well what happens with PMK glycidate and it’s various incarnations when it is hydrolysed? What’s produced? Does anyone actually know?
Yes, the conversion of PMK Glycidate to PMK does not have to be 100% efficient, which can leave PMK Glycidate in the mixture.
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.



See:
 
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Biscuit

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Dec 27, 1999
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Thank you. But what is the other part of the glycidate molecule that’s broken off to
Leave PMK behind? Is it Acetate ion/acetic acid? And does PMK glycidate always hydrolyze in the same way or might different bonds be broken leaving a bit of
MD phenylacetic acid? There seem to be a
Lot of variables especially as we have chiral centres in play and Methyl ethyl and other types of glycidates.

This is an interesting article as well, which shows a lot is being done on these compounds at the moment:

“Identification of specific markers for amphetamines synthesized from glycidic acid pre‐precursors and retrospective search in German profiling database“

https://onlinelibrary.wiley.com/doi/abs/10.1002/dta.2686
 

Biscuit

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Can you name the products? Looking messy to me. PMK, maybe MD PAA, acetate, that epoxide isn’t going to last.

I’m just hoping for clarity on glycidate hydrolysis —> PMK + ? + ?

What do you say the substance on the right is please?

I think it’s far more complex and inexact than the producers understand. Take this excerpt from book here, at bottom of first page, would be great to get the whole article...

https://pubs.acs.org/doi/pdf/10.1021/jo00832a021
 

ThreePointCircle

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Apr 21, 2016
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Obviously the silica on the TLC plates has to be similar to the one in the column.
Which isn't that easy. I was using pure silica in the column (wow that's expensive stuff btw), but the plates have the indicator and binders added. Tbf, the first set of plates had a hard layer with their binders, but my new bigger plates have a soft binder so maybe they are more similar.

I know the procedure is to then test all the fractions afterwards on tlc but I'm wondering how many column volumns to do and size of test tubes for fractions etc... I guess its about sitting down and doing the 1/rf but that assumes the plate and the column behave in a similar fashion.

BTW, thanks for the video link. I had found that once before and was looking for it.
 
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ThreePointCircle

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Apr 21, 2016
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I was just reviewing your experiments on the Wiki, @ThreePointCircle. Your experiments show the separation of two compounds. I just don't know how to proceed from there. Did you ever reach out to Wedinos about analyzing the plate? Drugs Data never replied to me about that.
I got bigger plates with the hope of getting a better separation and then approaching Wedinos. I've ran one with the same system but the rf was radically different (like 0.95 instead of 0.45 or whatever it was before). The bigger plates don't have a hard layer and are behaving very differently. So basically need to go back to playing with systems and everything, which probably means ordering some more solvents. I just haven't got round to it yet.
 
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