What is wrong with the MDMA available today? - v2

[vash445]

I llooked at the various syntheses and it appears that with the 'moonrock' MDMA, halogenation of the aromatic was the most commonly observed impurity.

But in all fairness, 'moonrock' does essentially mean nobody in the chain from producer to consumer can cut the stuff. In the 80s pill presses were hard to obtain and costly so those who made Doves (or whatever your favouroite was) had invested a considerable ammount in branding their product to keep up the value.

Then idiots would buy good pills, crush them, add a cut or just repress with less in each pill. So nobody really knew what they were getting and value collapsed. So someone has VERY cleverly solved this issue for now at least. SOMEONE will figure out how to adulterate moonrock...

"To the best of our knowledge, there are very few examples where a continuous-flow bromination has been developed that includes an in-line purification before telescoping into a subsequent reactor..."

Also please note, I understand this is norket via a-bromo (ketone) compounds or even potentially, B or y if you dig more. However, Conversion and yield were determined by

"1H NMR using 1,3,5-trimethoxybenzene as an internal standard Isolated yield." ...1,2,3-trimethoxybenzene to 1,3,5-trimethoxybenzene involves "Friedel-Crafts acylation" followed by a decarboxylation step then forward yields... well that isn't important here,

The importance here is for someone /anyone who doesn't know chemistry, and how it is related is that most reactions can sub bromo for iodo, etc. etc.

Anyways take a look at for reference

. _________ ________ proceeds via tricarbonyl(h6-1,2,3-trimethoxybenzene)chromium complex. Treatment of tricarbonyl(h6-1,2,3-trimethoxybenzene)chromium complex 1 with acetonitrile carbanion in THF and then with iodine followed by reduction of the nitrile function gives mescaline. Deprotonation of complex 1 at the C5 carbon with LiTMP followed by chlorination, bromation or iodation gives 5-chloro, 5-bromo or 5-iodo complexes, useful synthons in organic synthesis for the preparation of 1,2,3-trimethoxy-5-substituted derivatives, precursors of natural products. Hydrogenation of the nitrile 5 using a literature procedure [2g] gave me_ _ _ _ _ _ _ in 80% yield and in 66% overall yield starting from 1,2,3-trimethoxybenzene




Continuous processing is becoming increasingly attractive for the manufacture of medicines because it offers opportunities for faster process development and safer handling of hazardous reagents. (1) Over the past two decades, continuous-flow chemistry has become commonplace in both academia and industry and nowadays it pervades the whole process of research, from reaction discovery and optimization to scale-up and production of fine chemicals and active pharmaceutical ingredients. (2) The increasing interest in this field stems from the many advantages that synthesis in-flow can offer. Specifically, processes can often be made safer, greener, and more efficient when performed in continuous flow. These benefits are particularly apparent when working with hazardous materials, where the scalability of a process in a batch format can be problematic. (3,4) Flow chemistry also offers flexibility in reconfiguring reactors to adapt to changing manufacturing requirements. This is particularly useful in the context of personalized medicine, which leads to the production of a larger number of compounds but in relatively small amounts. In this paper, we demonstrate how flow chemistry can simplify the synthesis of norketamine (5), a pharmaceutically relevant metabolite of the antidepressant, ketamine (4). We take advantage of flow chemistry to minimize the risks of handling toxic reagents such as ammonia and molecular bromine on a kilo scale. In our experience, we found that the resultant crude mixture remained considerably colored following this protocol (an indication of bromine and/or its derivatives) and we were keen to develop a procedure that efficiently removed these contaminants. As such, several aqueous quench solutions were trialed."

A three-stage continuous-flow process for the synthesis of norketamine (5) is reported. Initially, α-bromination of the key precursor 1 was achieved with quantitative conversion using a CSTR that allowed the safe removal and quenching of the hydrogen bromide by-product. This process was demonstrated on a 0.89 kg/day scale. Next, the subsequent imination process was achieved in excellent yield, representing a rare example of the use of liquid ammonia in a continuous-flow reactor. It was then demonstrated that these processes can be linked via an in-line quench and purification with a liquid–liquid membrane separator. Finally, the last step in the synthesis of norketamine (5) was achieved on a 1.4 kg scale via the thermal rearrangement of the α-hydroxy imine 3 in a commercially available tubular flow reactor.

The product was not isolated but instead N-Boc protected for use in subsequent steps

See
Organic Process Research & Development
Cite this: Org. Process Res. Dev. 2022, 26, 4, 1145–1151

https://doi.org/10.1021/acs.oprd.1c00407

Copyright © 2022 American Chemical Society. This publication is licensed under


Published March 26, 2022 for more on telescopic (α-bromoketone)

At least how I read it.

 

[vash445]

"To the best of our knowledge, there are very few examples where a continuous-flow bromination has been developed that includes an in-line purification before telescoping into a subsequent reactor..."

Also please note, I understand this is norket via a-bromo (ketone) compounds. However, Conversion and yield were determined by

"1H NMR using 1,3,5-trimethoxybenzene as an internal standard Isolated yield." ...1,2,3-trimethoxybenzene to 1,3,5-trimethoxybenzene involves "Friedel-Crafts acylation" followed by a decarboxylation step then forward yields... well that isn't important here,

The importance here is for someone /anyone who doesn't know chemistry, and how it is related is that most reactions can sub bromo for iodo, etc. etc.

Anyways take a look at for reference

. Mescaline synthesis via tricarbonyl(h6-1,2,3-trimethoxybenzene)chromium complex. Treatment of tricarbonyl(h6-1,2,3-trimethoxybenzene)chromium complex 1 with acetonitrile carbanion in THF and then withiodine followed by reduction of the nitrile function gives mescaline. Deprotonation of complex 1 at the C5 carbon with LiTMP followed by chlorination, bromation or iodation gives 5-chloro, 5-bromo or 5-iodo complexes, useful synthons in organic synthesis for the preparation of 1,2,3-trimethoxy-5-substituted derivatives, precursors of natural products. Hydrogenation of the nitrile 5 using a literature procedure [2g] gave mescaline in 80% yield and in 66% overall yield starting from 1,2,3-trimethoxybenzene




Continuous processing is becoming increasingly attractive for the manufacture of medicines because it offers opportunities for faster process development and safer handling of hazardous reagents. (1) Over the past two decades, continuous-flow chemistry has become commonplace in both academia and industry and nowadays it pervades the whole process of research, from reaction discovery and optimization to scale-up and production of fine chemicals and active pharmaceutical ingredients. (2) The increasing interest in this field stems from the many advantages that synthesis in-flow can offer. Specifically, processes can often be made safer, greener, and more efficient when performed in continuous flow. These benefits are particularly apparent when working with hazardous materials, where the scalability of a process in a batch format can be problematic. (3,4) Flow chemistry also offers flexibility in reconfiguring reactors to adapt to changing manufacturing requirements. This is particularly useful in the context of personalized medicine, which leads to the production of a larger number of compounds but in relatively small amounts. In this paper, we demonstrate how flow chemistry can simplify the synthesis of norketamine (5), a pharmaceutically relevant metabolite of the antidepressant, ketamine (4). We take advantage of flow chemistry to minimize the risks of handling toxic reagents such as ammonia and molecular bromine on a kilo scale.


In our experience, we found that the resultant crude mixture remained considerably colored following this protocol (an indication of bromine and/or its derivatives) and we were keen to develop a procedure that efficiently removed these contaminants. As such, several aqueous quench solutions were trialed."

A three-stage continuous-flow process for the synthesis of norketamine (5) is reported. Initially, α-bromination of the key precursor 1 was achieved with quantitative conversion using a CSTR that allowed the safe removal and quenching of the hydrogen bromide by-product. This process was demonstrated on a 0.89 kg/day scale. Next, the subsequent imination process was achieved in excellent yield, representing a rare example of the use of liquid ammonia in a continuous-flow reactor. It was then demonstrated that these processes can be linked via an in-line quench and purification with a liquid–liquid membrane separator. Finally, the last step in the synthesis of norketamine (5) was achieved on a 1.4 kg scale via the thermal rearrangement of the α-hydroxy imine 3 in a commercially available tubular flow reactor.

The product was not isolated but instead N-Boc protected for use in subsequent steps

See
Organic Process Research & Development
Cite this: Org. Process Res. Dev. 2022, 26, 4, 1145–1151

https://doi.org/10.1021/acs.oprd.1c00407

Copyright © 2022 American Chemical Society. This publication is licensed under


Published March 26, 2022 for more on telescopic (α-bromoketone)

At least how I read it.

I also wonder, we all know that ketone can be made via an Enamine formation followed by oxidation. Pain in the rear due to single, double and triple octive oxygen ( of something like that. IE mechanical O2 vs synthesis of O2.. and with bromine, Br2 etc, very not fun to play with.. Instead I do also wonder if, The Bromination of Enaminones with N-Bromosuccinimide instead of the Enamine could be at play instead. Enaminones (which are nitrogenous compounds with a carbonyl group adjacent to a carbon-carbon double bond and an amine group) can be reduced to enamines or ketones

An efficient method for the preparation of β-amino-α,β-unsaturated carbonyl compounds is demonstrated. Bench-stable sodium 3-oxo-enolates were prepared from carbonyl compounds, and reacted with amines in the presence of an acid and a desiccant...3-oxo-enolates are specific types of enolates where the carbonyl group (C=O) is located at the 3-position of a ring or in a molecule. APPAN is 3-Oxo-2-phenylbutanenitrile. Methyl 3-oxo-2-phenylbutyrate (MAPA) is also recently circulating precursor a precursor of amphetamine and methamphetamine. MAPA has a hybrid chemical structure of acetoacetic acid ester and it's main ketone. Acetoacetic acid ester is de-esterified and decarboxylated to give the ketone by heating under acidic conditions; therefore. Considering that ethyl 3-oxo-2-phenylbutyrate (EAPA), methyl 3-oxo-4-phenylbutyrate (MGPA), and ethyl 3-oxo-4-phenylbutyrate (EGPA) have the same chemical features as MAPA, it is safe to assume these also exist as an MD version somewhere


So there is little doubt an MD version of 3-oxo-enolates is around. The 3-oxo-enolate can exist in two forms: the keto form (the ketone) and the enol form. The enol form has a double bond between the alpha-carbon and the carbon adjacent to the ketone, and an alcohol group attached to the alpha-carbon. If an enolate is formed from a ketone and reacts with another carbonyl (like a ketone), the resulting product is a 1,3-diketone or 1,3-ketoester if the second carbonyl was an ester. One could go many different routes to Ketones, For example, Bromine will react with the enol form, adding a bromine atom at the carbon bearing the enol double bond. This process can happen twice, resulting in a dibromo ketone for example I think? Solid and liquid 1,3-diketones and b-keto esters can be successfully and selectively brominated with NBS at room temperature with no solvent



Or that Manganese-Catalyzed Anti-Markovnikov Hydroamination of Allyl Alcohols via Hydrogen-Borrowing Catalysis is interesting in that


Additionally, the allyl alcohols, synthesized from the monoterpenoid citronellal (6a) and the commercially used fragrant helional (6b), could also be functionalized under the manganese catalyzed hydroamination conditions and the products 7a,b were isolated in high yields, and moderate diastereoselectivities (Scheme 2c). Additionally, cytisine 2zh could be hydroaminated with the allyl alcohol derived from helional (6b), yielding the conjugate 7c in moderate 50% yield.

I imagine the Cyclization breaking could be opened, but I'm not sure though, I'm sure those that know, would know what I'm alluding to. IE ring opening of the epoxides, Heck, Suzuki, and Olefin Metathesis Reactions but i'm probably more wrong here then uptop.

Of course, there is a DOI for a process leveraging the chiral pool has been developed to access enantiomers of both MDA and MDMA. Critical aspects of the process were identified and include utilization of freshly prepared Grignard solution (3) with rapid addition of this solution to aziridine 6 and subsequent shortened reaction times. Characterization data have also been provided to enable in-process monitoring for key reaction intermediates as well as critical and noncritical byproducts with consideration of their impact on final product quality

I also removed a lot of information to obey the rules here. And take my thoughts with a grain of N-BOC MDMA.hcl salt this is probably way out of my wheelhouse but, I feel there could be some valid in sites here

 

[unodelacosa]

"Sit back and have a cup of Joe and watch the wheel go round, 'cause those damned blue-collar tweekers, they have always run this town…" – Les Claypool

But in all fairness, 'moonrock' does essentially mean nobody in the chain from producer to consumer can cut the stuff. In the 80s pill presses were hard to obtain and costly so those who made Doves (or whatever your favouroite was) had invested a considerable ammount in branding their product to keep up the value. Then idiots would buy good pills, crush them, add a cut or just repress with less in each pill. So nobody really knew what they were getting and value collapsed.

Very true. I watched the same thing happen in the U.S. during the 90s. However…

So someone has VERY cleverly solved this issue for now at least. SOMEONE will figure out how to adulterate moonrock...

Exactly. I don't think it was as clever as you're giving them credit for… I think this is just how someone's weird synthesis went down and wound up. And then they were like, umm, Moon Rocks! Yeah that's what we'll call it. And a star was born. Or a moon rather. Selah.

 

[4DQSAR]

Exactly. I don't think it was as clever as you're giving them credit for… I think this is just how someone's weird synthesis went down and wound up. And then they were like, umm, Moon Rocks! Yeah that's what we'll call it. And a star was born. Or a moon rather. Selah.

I can almost 100% bet the chemists never came up with the term 'moonrock'. I did suggest that it was likely a solvent-free route so yeah, the product may well have come out in big chunks but people who do this sort of thing at scale don't bother with nicknames. To them, it's just product.

On a practical level, a single huge crystal is going to have a higher density than a powder so it's more likely something as pragmatic as making the product as small and easy to smuggle as possible and possibly in the past vendors were crushing up those rocks to make a powder until one of them decided that not only did they not need to, but in fact it was an asset - a way to assert that your product is uncut.

But I guess anything is possible.

 

[unodelacosa]

I can almost 100% bet the chemists never came up with the term 'moonrock'. I did suggest that it was likely a solvent-free route so yeah, the product may well have come out in big chunks but people who do this sort of thing at scale don't bother with nicknames. To them, it's just product.

Oh I don't know, man. Having chemistry chops and marketing acumen aren't mutually exclusive, you know. Who's to say, and it's beside the point.

but in fact it was an asset - a way to assert that your product is uncut.

That's an interesting theory. Feels like you might be giving them too much credit, but I'll admit I'm out of my depth when it comes to large scaled up production. But in my best personal conjecture I think it's more likely just the result of the chemists putting in less effort to churn out more product, and who has time to break up the crystals? Tag it, bag it, sell it to the butcher in the store. And Robert is your mother's brother & all that clever British word play.

It seems like It's just another form of "re-rock" but with MDMA, to me. You seem to be well trained/educated in organic chemistry on the larger scale production side, so I'll defer to your judgment.

 

[4DQSAR]

It seems like It's just another form of "re-rock" but with MDMA, to me. You seem to be well trained/educated in organic chemistry on the larger scale production side, so I'll defer to your judgment.

I'm a medicinal chemist with a tiny little microscale setup in my home. When a drug discovery team is working on a new project, yield doesn't matter much and cost is mostly in HAVING a lab with all of the tools that allow anything (within reasonable limits) to be synthesized.

But once a new candidate is patented, it's the job of chemical engineers to find the very cheapest way of making a specific compound. So while my education and experience is adjascent to this sort of thing, it really is a seperate disipline.

I know enough about it to know I really don't know MUCH about it.

I DO recall seeing the GC-MS and NMR data on 'purple moonrock' and it turned out that ring halogenation products were the main impurities. Both iodination and chlorination. That strongly suggests a specific route and I think what is interesting is that it's also just about the cheapest route BUT does require an initial investment in an appropriate reactor. So I think someone was/is playing the long game. As chemical engineers do, they will tweak the reaction to avoid impurities.

BTW it's an open secret that certain Chinese companies are deforesting regions of Cambodia & Burma and that would include trees whose oils contain a lot of safrole. But AFAIK nobody has actually been able to join the dots.

I just think it LOOKS very Chinese. Not an insult - they are the masters of keeping down costs.

 

[unodelacosa]

Here's a Pepsi challenge I have for anyone on this thread who believes that something is wrong with today's MDMA. Try some 5-APB if you can find it. Personally, I like it better than MDA and MDMA. I think it hits hardAF and last longer plus has maybe a third the amount of hangover. It's more like MDA than MDMA, but the stuff makes me roll my fucking tits off. It belongs to a class of drugs called the benzofurans and they include 5-APB, 6-APB and their n-methylated counterparts, 5-MAPB and 6-MAPB. Of them, personally I've tasted 5-MAPB and a combination roll of 5-MAPB and 6-MAPB, but they pale in comparison to 5-APB which is remarkably euphoric.

certain Chinese companies are deforesting regions of Cambodia & Burma

Still? I thought the new hot spots for this were in Northern Africa.

I understand in Afghanistan they're growing Ma Huang (the ephedra plant) for meth production now in addition to opium… Evidently the climate is just right.

I once vac distilled dill apiole from Indian dill seed oil and used that make DMMDA-2 and DMMDMA-2, which were both interesting compounds that are exceedingly rare for some reason. Oddly though, DMMDA-2 is mentioned in David Foster Wallce's infinite Jest where he refers to it as "Starry Night". There's also the drug MMDA which is described in PiHKAL as being capable of manifesting "mind movies" out of one's own memories in their head. I've had hints of this effect in other psychedelics and would like to explore this. Maybe one day.

But yeah: 5-APB. Try it and see if that's not a return to magic. I'm curious to hear others' thoughts on this compound.

 

[vash445]

Here's a Pepsi challenge I have for anyone on this thread who believes that something is wrong with today's MDMA. Try some 5-APB if you can find it. Personally, I like it better than MDA and MDMA. I think it hits hardAF and last longer plus has maybe a third the amount of hangover. It's more like MDA than MDMA, but the stuff makes me roll my fucking tits off. It belongs to a class of drugs called the benzofurans and they include 5-APB, 6-APB and their n-methylated counterparts, 5-MAPB and 6-MAPB. Of them, personally I've tasted 5-MAPB and a combination roll of 5-MAPB and 6-MAPB, but they pale in comparison to 5-APB which is remarkably euphoric.


Still? I thought the new hot spots for this were in Northern Africa.

I understand in Afghanistan they're growing Ma Huang (the ephedra plant) for meth production now in addition to opium… Evidently the climate is just right.

I once vac distilled dill apiole from Indian dill seed oil and used that make DMMDA-2 and DMMDMA-2, which were both interesting compounds that are exceedingly rare for some reason. Oddly though, DMMDA-2 is mentioned in David Foster Wallce's infinite Jest where he refers to it as "Starry Night". There's also the drug MMDA which is described in PiHKAL as being capable of manifesting "mind movies" out of one's own memories in their head. I've had hints of this effect in other psychedelics and would like to explore this. Maybe one day.

But yeah: 5-APB. Try it and see if that's not a return to magic. I'm curious to hear others' thoughts on this compound.

Yes the APB are around but still lots of meh on the succient form then HCL.

This was discussed about 1-2 pages back and a post from borax 12 years ago meh 6apb/benzofuran is around and ULTRA pure stuff is the tits

I've been recrystallized MDMA and the Honey has now reached BLACK. I can definitely smell and see black carbon during removal. The previous MDMA looked brown and I was about to labtest. But I'm like let's try some acetone and ethanol washes first before one last recrystallization.



The MDMA still looks gross but not at least something you would buy on the streets. But my goal is to have the gross black test as something other MDMA.

 

[unodelacosa]

This was discussed about 1-2 pages back and a post from borax 12 years ago meh 6apb/benzofuran is around and ULTRA pure stuff is the tits

If you're referring to Borax's proposed drug combo, "Polly", yes I've made several iterations of that, and none of them are like MDMA in my opinion. Better off going with 5-APB as far as I'm concerned. But hey, that's just me. YMMV, as always.

I've been recrystallized MDMA and the Honey has now reached BLACK. I can definitely smell and see black carbon during removal.

Say what?

The previous MDMA looked brown and I was about to labtest. But I'm like let's try some acetone and ethanol washes first before one last recrystallization.

Um, ok. …

The MDMA still looks gross but not at least something you would buy on the streets. But my goal is to have the gross black test as something other MDMA.

Why is there gross black shit in your the MDMA you have? That's a little suss, isn't it?

 

[vash445]

If you're referring to Borax's proposed drug combo, "Polly", yes I've made several iterations of that, and none of them are like MDMA in my opinion. Better off going with 5-APB as far as I'm concerned. But hey, that's just me. YMMV, as always.


Say what?


Um, ok. …


Why is there gross black shit in your the MDMA you have? That's a little suss, isn't it?

No not his poly combo



Consistency in dosing - the succinate salt form typically contains a LOT more succinate than it should. There was certainly no lack in demand - the pilot batches were universally reported as being better.

The general market. The vendor I was speaking to said their best batches contained ~20% 4-APB because the only way to remove it was through chromatography which is very uneconomical. He speculated that its presence might be the reason it was so hard to crystallise.

A large quantity of vendors also had serious excess of succinic acid present in both 6-APB and 5-APB, well up and over 50% of resulting powder.

It is the reason that a lot of people seemed to find 5-APB.hcl substantially stronger at what should have been equipotent doses. (taking into consideration what % of both powders should have been 5-APB, and adjusting the amount consumed to contain equal amounts of 5-apb).


edit: also in talks i've had with a few vendors most have said that 6-APB (for some reason, unknown to me) simply was not stable in base form... perhaps the 4-APB *contaminant* could've been to blame.

Yup, same thing was happening with 6-APB's succinate content and even the fumarate content of some of the tryptamines we analysed.

I had no idea market 6-APB was so impure. Glad I haven't touched the stuff in a long time. Is succinic acid used here as a cut? I don't see a use for it here as a reagent but my organic chemistry knowledge is limited.

https://www.reddit.com/r/DrugNerds/s/S4dz29C8ym

 

[vash445]

If you're referring to Borax's proposed drug combo, "Polly", yes I've made several iterations of that, and none of them are like MDMA in my opinion. Better off going with 5-APB as far as I'm concerned. But hey, that's just me. YMMV, as always.


Say what?


Um, ok. …


Why is there gross black shit in your the MDMA you have? That's a little suss, isn't it?

Well it's wasn't pure white MDMA I started with so it's not that odd little color spread over a lot of crystal. But yes I suspect this is sub 1-2% impurities Rick Doblins from MAPS said you need REALLLY PURE drugs with Joe Rogan the other day. And the "Dallas crew" was mentioned...!

Bromine? Carbon? You tell me? Went from purple or brown MDMA to this slop. I can definitely smell, see etc over time I first smell and see safrole, ketone etc oil seperation,

then later Chromium or some kinda orgmetal, like magensium etc.... later deffiently carbon maybe Carbon on black now or charcoal for purification. Etc etc

The possibility of using carbon black (CB) as a support of palladium catalysts for the selective hydrogenation of organic compounds is considered. The advantages of Pd/CB catalysts are demonstrated by examples of liquid-phase hydrogenation of aromatic aldehydes and nitro compounds. The combination of high catalytic parameters (activity, selectivity, and stability) achieved by these catalysts in hydrogenation reactions indicates that they are promising for use on an industrial scale, in particular in the syntheses of fine chemicals.

MDMA was either brown, green or pink or purple before recrystallization.

Slop is now officially "black". When before it was more "brown" and smelt of SAFROLE/ketone. I'll see if I could pull any MDMA later. Then send the slop for analysis when I don't think MDMA might interfere with it anymore.

 

[vash445]

 

[vash445]

Labor of love to now see if I can turn "junk"

Into magic

 

[vash445]

BTW the problem will come when a competing group adopts the same methodology as those producing moonrock - this it inevitable.

Finding a vastly cheaper way of making something is a GREAT way to make a lot of money in the short-term. But as soon as competition arrives, people who are prepared to forego profit to establish a market-share will sell the product at cost (or close to it). At 'pennies per dose', to make money, the scale has to be huge.

The fact that methamphetamine can be made from glycidate esters but we haven't seen the price of that collapse does re-enforce the detail that safrole is the precursor.

If someone were to find a dirt-cheap source of allylbenzene, meth would likewise cost pennies per dose. But that hasn't happened (AFAIK) which sugggests pseudoephedrine or maybe L-PAC are now the common precursors for that compound.

BTW L-PAC is legal and produced on vast scales via genetically modified yeast converting benzaldehyde IS interesting as 3,4-MD L-PAC would, in theory, offer another precursor.

If someone were to find a dirt-cheap source of allylbenzene, meth would likewise cost pennies per dose. But that hasn't happened (AFAIK) which sugggests pseudoephedrine or maybe L-PAC are now the common precursors for that compound.



Meh I doubt it...

[novel synthesis route] Method for making pharmaceutical compounds D meth US20100125146A1-20100520-C00001​

wonder how they lately made dextro-meth or amph (ICE or speed direct, without racemat DL- separation)...

CAS 16251-45-9 from .... (No sourcing ) (can only be bought in minimum 2.5 Kgs drum, price 844 USD/Kg), methylate it (super simple), then hydrogenation that intermediate 4 hrs, super fast simple ulra clean non-hazard non-contaminated reaction at only 2 atm, 90-95% yield.

https://patents.google.com/patent/US20100125146A1/en

the reduction is carried out using gaseous hydrogen and a catalyst. (I wonder if borohydride or stab would work or even feeding hydrogen gas directly with such a catalyst or similar such as cyclohexane?)

In a preferred embodiment, the catalyst is palladium on carbon. However, there are alternative means of carrying out the reducing step. Such means may include carrying out transfer hydrogenolysis using hydrogen donor agents such as readily dehydrogenatable hydrocarbons, (e.g. methyl cyclohexene), formic acid, ammonium or potassium formate, and hydrazine (Brieger G, Nestrick T, J. Chem. Rev., 1974, 74, 567-580). The skilled person will appreciate that other means of carrying out the reduction may also be used

The first 3-4 look cheap and readily available I would avoid the last one.

(4R,5R)-4-Methyl-5-phenyl-2-oxazolidinone is an intermediate in the synthesis of (-)-Pseudo Norephedrine

As (4R,5R)-4-Methyl-5-phenyl-2-oxazolidinone is an intermediate in the synthesis of (-)-Pseudo Norephedrine


Oxozolones are not difficult to prepare .....java

Methods for synthesis of Oxazolones: A Review

http://www.sphinxsai.com/Vol.3No.3/Chem/pdf/CT=17(1102-1118)JS11.pdf

A related patent.

http://www.google.com/patents/US3029189

Kinetic and mechanistic studies of the Dakin-West reaction Norman L. Allinger , Grace L. Wang , Brian B. Dewhurst J. Org. Chem., 1974, 39 (12), pp 1730–1735 DOI: 10.1021/jo00925a029

......with some creative evaluation, the correct combination can be made to acquire the target compound, along with insights from patents provided by Baba_McKensey it' doable.....it seems to me........java

More food for thought: http://www.organic-chemistry.org/synthesis/heterocycles/oxazolidinones.shtm The first one lets us know why the patent method works: condensation of a substituted ethanolamine with urea with catalytic nitromethane under microwave irradiation (G. Bratulescu, Synthesis, 2007, 3111-3112 in case the link goes bad). That substituted ethanolamine would have to be (1R,2S)-PPA or ephedrine

 

[vash445]

Now if P2P OR MD-P2P is the goal to stay on topic...

the third alert raised awareness of the identification of a new designer precursor of MDMA and related “ecstasy”-type substances,
the sodium salt of isopropylidene (2-(3,4-methylenedioxy-phenyl)acetyl)malonate (IMDPAM)

an alternative synthesis method which is allow to get Phenylacetone (P2P) and PPA from Diethyl(phenylacetyl)malonate. This method consist of Diethyl(phenylacetyl)malonate alkaline hydrolysis into Phenylacetyl-malonic acid sodium salt with subsequent hydrolysis by cheap and easy available hydrochloric acid.

Some bees buzzed that diethyl(phenylacetyl)malonate could be used directly in a Leuckart reduction without first being converted to P2P..

Around 100 euro per kilo for the malonate( less considering shipping was included) 800g yields
200g P2P and 200g PAA yield is 52% are obtained

OR 71% JUST p2p



Of course also a simple route to 3-oxo-4-phenylbutanoic acid be malonate ester synthesis? You react phenyl acetyl chloride with diethyl malonate. Upon decarboxylation and hydrolysis, you will get the 3-oxo-4-phenylbutanoic acid, which can be further decarboxylated to p2p. It seems rather easy if you can not get Ethyl 3-oxo-4-phenylbutanoate.

 

[4DQSAR]

Well, there seems no shortage of PMK. There is a whole group of people who don't make product - they just make PMK.

Don't know how the law stands on that, Unless it's proven that the seller KNOWS what it's being used for, not much AFAIK since I haven't read of any of those people being busted (on any major scale).

I guess the same is true for fentanyl in Mexico. While the precursors are 'controlled', Chinese sources now sell the pre-precursors and I suspect that likewise there are people making the direct precursors but not the active and again, I suspect you have to prove intent.

 

[vash445]

Well, there seems no shortage of PMK. There is a whole group of people who don't make product - they just make PMK.

Don't know how the law stands on that, Unless it's proven that the seller KNOWS what it's being used for, not much AFAIK since I haven't read of any of those people being busted (on any major scale).

I guess the same is true for fentanyl in Mexico. While the precursors are 'controlled', Chinese sources now sell the pre-precursors and I suspect that likewise there are people making the direct precursors but not the active and again, I suspect you have to prove intent.

Of course ...

I just found it interesting

With reference to Article 1 of the Establishment Decree Expert Group Drug Precursors

(Establishment Decree), the Expert Group Drug Precursors hereby reports to the Minister of
Justice and Security and to the Minister of Health, Welfare and Sport on the substances described in the
appendix, namely:
-DEMDPAD
-IPAM
With regard to IMDPAM, it is noted that this substance has been included on the
Voluntary Monitoring List as of August 2023, which means that reporting on this substance is no longer necessary, given Article 1 paragraph 3 Establishment Decree.

Illegal manufacture of narcotics (Article 3 paragraph 4 sub a Establishment Decree)
- The substance DEPAPD is a precursor for BMK and registered pursuant to Regulation 273/2004 and R egulation 111/2005. When DEPAPD is substituted with a methylenedioxy ring (MD), the substance is DEMDPAPD, which is a precursor for PMK. PMK is a precursor for MDMA, included on
List I of the Opium Act. DEMDPAD can therefore be used for the illegal manufacture of narcotics.
In view of this and the discovery of the salt of DEPAPD in the Netherlands in the summer of 2022, it is expected that DEMDPAD can be found in the Netherlands in the near future.
- A salt of IMDPAM was found on 3 February 2023 in Dodewaard at a drug production location. IMDPAM is a precursor for PMK. PMK is the precursor for MDMA, included on
List I of the Opium Act. IMDPAM can therefore be used for the illegal manufacture of
narcotics. IMDPAM has been included on the Voluntary Monitoring List as of August 2023.
IPAM is a variant of IMDPAM, without the MD ring. IPAM is a precursor for BMK. BMK is a
precursor for amphetamine, included in List I of the Opium Act. IPAM can therefore be
used for the illegal manufacture of narcotics.
It is expected that IPAM - given the discovery of IMDPAM - can be found in the Netherlands in the near future.

 

[4DQSAR]

There will ALWAYS be a next precursor, sad to say.

L-PAC is the obvious one for meth and there are some odd holes in the laws surrounding ring-substituted amphetamines, Some loopholes.

 

[vash445]

Well, there seems no shortage of PMK. There is a whole group of people who don't make product - they just make PMK.

Don't know how the law stands on that, Unless it's proven that the seller KNOWS what it's being used for, not much AFAIK since I haven't read of any of those people being busted (on any major scale).

I guess the same is true for fentanyl in Mexico. While the precursors are 'controlled', Chinese sources now sell the pre-precursors and I suspect that likewise there are people making the direct precursors but not the active and again, I suspect you have to prove intent.

One the one had they have to prove intent. I could be making and documenting 1-(3,4-methylenedioxyphenyl)-2-butanone 3,4-methylenedioxy-2-methylaminobutane but really just tweak something so to speak.

On the other hand. It really depends on

The country (if USA state or federal charges) and the ammount of evidence

Eitherway expect the prosecutor to say

1) you were making meth and or MDMA even if it was a cathIone or bromo MDMMA. EXPECT THEM TO SAY It was also meth reguardless.

2) expect them to say you were making explosives because you have let's say an oxidizer, hexamine, and or aqua regia ( the last for processing motherboard gold) and that was your intent.

Oh you weren't making drugs. Then it was BOMBS, the prosecutor will tell the judge.

You go no it wasn't either. And they will still push you were drug manufacturer

Because you had

1) a propane tank (with sulfur not the expensive stuff for hash oil)

2) already been vape weed that you wash the nasty out it's THC is so low it's best for edible

3) that even IF were NOT making meth, or bombs. THE DA/ADA will say you were still making drugs ( with propane with sulfur and already vaped weed. Their (expert cop testimony will say)

4. We came upon what OUR experience is a METH LAB, BOMB FACTORY and a HASH OIL LAB

It is our experience that

A) these chemicals/items could be used in the manufacturer of drugs or bombs

B) our experience shows that "super labs" would
Have a ketone or aldehyde and would take a similar process.

C) We have dismantled 100s of meth labs and hash oil labs. Forget that the propane had sulfur and the weed was less then 3% THC/CBD.
Forget that your goal was ...

1-(3,4 methylenedioxyphenyl)-2-butanone or 3,4-methylenedioxy-2-methylaminobutane

The DA will say the LAB reports tested as meth or MDMA or that your attempt was to make... . And no matter how much you try to argue that GC/MS IS NOT ACCURATE

and that you need a NMR COSY, TOSY,C-13, H-1 AND HPLC and to compare the NMR of MDMA and meth to compare the charts. (Do you think your peer(s) is a chem major?)

Cuz the DA is just gonna say our "expert" has read the graph and has stated NMR and all tests like GC/MS is subject to interpretation. In our opinion he was breaking the law because

Our GC/MS came up MDMA, the NMR shows an "MD ring" and he attempted to make MDMA similar to "Bayer village" to meth ...

If it's state, you'll face all that shit

If it's federal they litterly have an even greater budget, and a lower lose rate

 

[4DQSAR]

Funny that (R) 7,α DMT (R) 7-methyl AMT) fully substitutes for MDA but doesn't appear to be explicitly controlled.

There will always be a way and what concerns me is that producers will be reduced to misrepresenting the product.

In the city where I grew up there was a cluster of deaths due to a batch of what was represented as MDMA. It was in fact a mixture of p-TAP and amphetamine. I PRESUME because some idiot thought they had found a cheap way to 'estimate' MDMA.