@vash445
It's worth reading the above paper. It explains that with only a single exception, all of the impurities previously found in MDMA hydrochloride are easily removed using an A/B (acid-base) extraction. The exception is a class. MDMA derivatives that have chlorinde and or bromine ions on the aromatic ring.
So they become part of the very MDMA molecule itself and would require an extremely costly and complex seperation technique to remove. Of course, it's hard to know what the subjective effects of 2-bromo MDMA, 5-bromo MDMA or 6-bromo MDMA are. Chlorine ions have also been detected:
postimg.cc
So:
3 monosubstitutions
2 disubstitutions
1 trisubstitution
But double that because the -Br ions can just as easily be -Cl ions. Then consider the mixtures of disubstitutions (8) and trisubstitutions (8) and in fact, that's a LOT of different impurities.
I think that's a very important detail. It seems like MDMA producers are going from precursors to pre-precursors and now to pre-pre-precursors.
I've since looked at a lot of vendors quoting a purity of the product (monrock). I was originally confused because the pure white microcrystals that were common in the late 1980s and early 1990s were essentially 100% pure. Because producers performed the proper A/B (acid-base) extraction that would remove safrole, isosafrole, piperonal, PMK or any of the reagents that were carried through to the final workup. So now I see moonrock on offer with the purity stated as being anywhere from 92% to 96%. It's none of those intermediates I mentioned that are ending up in the products, it's the brominated or iodinated derivatives OF MDMA that are present.
That would also explain the differing colours. The C-Br and C-Cl bond-lengths differ and differ again depending where they are on the rings and what other ring-substitution is present.
I should add that if a laboratory is prepared to srart from benzodiozole, it's a LOT more work:
Benzodioxole + Bromine ---> 5-bromo-
2H-benzodiaxole (which will also dibrominate to the 5,6-dibromo, tribrominate or even tetrabrominate). But all of those will then undergo.
1) 5-bromo-
2H-bromodioxone (or homologues) + Magnesium metal ---> 2-methyloxirane ---> 1-(
2H-1,3-benzodioxol-5-yl)propan-2-ol (or homologues)
2) 1-(
2H-1,3-benzodioxol-5-yl)propan-2-ol + NBS (N-bromosuccinamide
or TEMPO + Bromine
or sodium hypochloride ---> PMK
There are two important things about rhe above. It's only practical at large scales and it involves the use of bromine in two routes and I GUESS that sodium hypobromite would also be possible and if you already have need for bromine gase (very toxic), simply adding bromine to sodium hydroxide solution would produce sodium hypobromite so it would reduce the price slightly. But ring-chlorination of samples has been seen, so clearly sodium hypochloride is used, at least sometimes.
Now right up to the point where PMK is produced, all of the above is legal. I also note that both piperonal and PMK can both be used to produce PMK glycidate. It's entirely possible fo the two synthetics stesps in which first piperonal or PMK are produced and the step to prodice the legal PMK-glycidate are carried out in a single reaction vessel. I'm not an expert in chemical enginerting but it may be that instead of a batch process, the syntheis uses a continuous flow process so even if the police were to visit the production line, they would only even find small quantities of controlled precursors as they are made and converted into a legal intermediate in the same system.
But given the syntheis explained by the paper, even if ONLY 3,-4-methylendioxy <ring halogenated> methylamphetamines are in the product, that's a possible total of 62 compounds.
Unlikely to be present in toxic amounts, but THAT is why we are seeing HUGE crystals. When being taught organic chemistry, it's repeated that ONLY pure(ish) samples will form crystals and the melting-point and melting-range of the crystal gives an insight into the purity. The higher the melting-point and the smaller the range over which the crystal melts is considered a spot-check for purity.
But if my other theory ic correct, manufacturers are producing MDMA hydrochlorideand the final step is the heating of the product to above it's melting-pount (either under a vacuum or using a protective atmosphere such as dry nitrogen) to remove ALL of the other types of impurity and then allowing the product to slowly solidify. If one is considering blocks weighing many kilograps, it will inhernetly be slow, but it's possible that the heating and cooling is carried out in an insulated vessel. After all, if all you have to to is to leave it to stand for 24 hours, is that a problem?
I would love to know just what scale these labs are working on. Whoever has managed to achieve a route that at once avoids the legal control of precursors, provides for large-scale prodution and a route that allows semi-skilled workers to carry out production.
But as you said - the colour surely WILL tell you exactly what impurities there are in a sample. It's possible to calculate the bond-lengths for every C-Cl and C-Br bond so it's possible to take the date used to produce
figure 2 and to find use it to find how much of each impurity is present and therefore have a pretty good idea of which factory produced the sample.
That is one of the few advantages of following Shulgin's route and repeating the extraction process twice or even three times. If your product truly is 100% MDMA hydrochloride, it's chemically identically to eavery other sample of 100% pure MDMA hydrochloride. Yes, microcrystals, packaging and other forensic techniques can be applied, but the drug itself tells no takes.
Sorry to have gone on about if for so long. NOW I understand. Someone has found a route that makes the use of pre-pre-precursors a facile and dare I say it even a CHEAP route to make MDMA.
Amazing to think that in 1988 I used to pay £20 for a single 125mg MDMA tablet. But it was exactly that. What these people have been able to to is to reintroduce that potency but at a lower cost.
BTW I suppose the untimate would be for someone to produce (R) 7,α-DMT (7-methyl AMT). It's around four times the potency of MDMA and most people couldn't tell the difference between the two. For a while it was sold in Kokopelli as 'Empathy' but Dutch law changed.