@Gaffy – you're talking about the sodium cyanoborohydride reduction from MDP-2-P and the use of Palladium II Chloride as a metal catalyst in some form of oxidation. The p-benzoquinone Wacker oxidation really limits the amount of necessary (and expensive) Pd2Cl, but I think Shulgin took the performic acid route from isosafrole, no? And anyway, Al/Hg amalgam with methylamine either separately obtained or created in situ is an elegant reaction suffering only from having to work with deadly poisonous Mercuric chloride salts.
@indigoaura – ok first off, where are the references in this Wikipedia article? Lots of statements made, no sources given for them. "[MDMA] synthesized by methylation of MDA using methylating reagents such as methyl iodide" … this, to me, does not seem like it would happen too often as a realistic approach to manufacturing MDMA, not when so many other options exist for producing a methylated amine. Sure, it would reveal the method used, I suppose, and it does seem like excess reagent + excess heat would lead to this dimethylated formation, but I'd have to see evidence and actual numbers before I would believe this happens any kind of frequently.
Secondly there isn't exactly a wealth of information out there vis-à-vis the subjective effects of MDDM and how they combine with MDMA's effects. It's an interesting theory to consider, but it's far from conclusive.
Note that in this article they are referring to 3,4-methylenedioxy-N,N-dimethylamphetamine as MDDMA.Starting with 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N,N-dimethylamphetamine (MDDMA) and 3,4-methylenedioxy-N,N,N-trimethylamphetamine (MDTMA) were prepared. We evaluated the functional activities of the compounds at all three monoamine transporters in native brain tissue and cells expressing the transporters.
Our results suggest that the 3,4-methylenedioxyamphetamine analogs bind at the monoamine transporter orthosteric binding site by adopting one of two mutually exclusive binding modes. 3,4-methylenedioxyamphetamine and 3,4-methylenedioxy-N-methylamphetamine adopt a high-affinity binding mode consistent with a transportable substrate, whereas MDDMA and MDTMA adopt a low-affinity binding mode consistent with an inhibitor, in which the ligand orientation is inverted. Importantly, MDDMA can alternate between both binding modes, whereas MDTMA exclusively binds to the low-affinity mode.
Therefore, it can be assumed that MDDM was present as a synthesis by-product or impurity in the “ecstasy” tablets taken by the victim. Gimeno et al. substantiated that MDDM can be formed during the clandestine manufacture of MDMA by reductive amination of 3,4-methylenedioxyphenyl-2-propanone (MDP2P) by dimethylamine [20, 21]. This MDDM formation takes place because of the presence of dimethylamine as a contaminant in methylamine .
I've been thinking this subject over a bit before responding and thinking about the synthesis, especially from the perspective of a clandestine chemist acquiring a bulk shipment of PMK-glycidate, and what that would entail in terms of processing that quantity.We were talking about MDDMA in the original thread in relation to the NMR results shared by Vash. I know that situation got weird, but assuming those NMR results were valid, remember how we were trying to figure out what the additional peaks were? We compared the peaks to published data and were speculating that it looked a lot like MDDMA. Check the posts from around #3661, or just do a search for MDDMA and they will all appear.
Well my first thought was perhaps a very careful, arduous, fractional vacuum distillation. But it's likely the boiling points might still be too close. Let's see, I'm cracking open my copy of The Shulgin Index to look up the entry on MDDM (or as it's listed in the book, MDDMA).If anyone knows how MDMA could be successfully separated from MDDM, let me know.
Structural homologues were separated by liquid chromatography (Noggle et al., 1987a) and LC/CS (Noggle et al. 198
Well my first thought was perhaps a very careful, arduous, fractional vacuum distillation. But it's likely the boiling points might still be too close. Let's see, I'm cracking open my copy of The Shulgin Index to look up the entry on MDDM (or as it's listed in the book, MDDMA).
MDDMA freebase's boiling point is listed as "85-88 °C/0.15 mm (Braun et al., 1980)".
Meanwhile MDMA freebase boils at "100-110 °C/0.4 mm."
Maybe don't totally rule that one out. However, in the same reference manual under the entry for MDDMA, it notes:
I'm thinking a proper chromatography column is what you would need. Not "high performance" or "GC-MS", just simple separation…
I've seen reports that used Methanol/DCM mixture as a solvent for column chromatography, ratio was 90% DCM and 10% Methanol. Also recommended to perform an acetone wash to your MDMA sample before purifying it with column.Thank you for your replies.
"I'm thinking a proper chromatography column is what you would need. Not "high performance" or "GC-MS", just simple separation…"
Everything seems to keep coming back to this. Column chromatography is part of the MAPS process of purification, and other users have speculated this is what is needed to truly get good results.
I have gone back and forth about buying what is needed to complete the chromatography myself. However, there seems to be a lack of clarity regarding which solvent would work best. Until I have an accurate idea of which solvent to use, I am hesitant to proceed with a costly operation. If I knew for certain that it would work, then I would make the investment. Do you have any suggestions regarding which solvent to use in a column?
"But there are numerous possibilities for accidental co-synthesis of active impurities associated with different synthetic routes. "
Yes. I have seen this in many research articles, and even MAPS references the phenomenon when providing an overview of their synthesis process. They discuss that ambient temperature can impact the result in significant ways.
Update from International Energy Control.
They were unable to quantify the 3,4-methylendioxy-N,N dimethylamphetamine because they do not have the standard for it. I asked if it would be possible to donate the standard so quantification of this impurity would be possible. They are looking into that now, and they are going to let me know what the cost would be.
My plan going forward is as follows:
-Donate the standard for 3,4-methylendioxy-N,N dimethylamphetamine to IEC
-Submit additional meh samples
If my hypothesis is correct, then I would expect to see the same/similar impurity in other samples. I hope that if multiple samples with subpar effects contain the same impurity then perhaps I may be more able to gain the attention of a researcher or university.
I have one of those, and the lighter test is far easier to read. The main problem was that I melted some down, it turned out to not be what I had paid for, and I did it anyway. ONLY pure MDMA melts into a blood-red puddle. Meth melts clear. A combination of the 2 could certainly have produced a semi-translucent yellow. But anyway, I'm not going to be seeking or purchasing any "MDMA" for a long time.If the issue is getting sold meth, your problem could be easily solved by replacing your lighter with a $20 vial of the Marquis reagent.