r/TheeHive

Tollen's and melons, removing that tricky residual aldehyde

Tollen's and melons, removing that tricky residual aldehyde

So I have been playing with enamine > ketone. I have done it successfully plenty of times. BUT I pretty much always have residual traces of aldehyde remaining. Sometimes more of a "trace" than other times. This last time has turned into quite the debacle.

I usually get pretty damn close to complete conversion but never 100%. When I distill the ketone I use a column and bring the temp up VERY slowly. Even if there is some isolation, anyone who's done this knows distillation just won't work to separate them.

My next bright idea was DCVC. I can achieve good seperation on a plate so why not run it through a column. And in theory I know I could make this work. I've never done DCVC but it is an opportunity to learn some new skills. And I did try two times on a small sample.

While I failed to get seperation on my 2 test runs I know it is doable and know what my issue was, most likely. My test runs were somewhat proportional to what my big run would be. The issue is overloading which is why I picked DCVC. Supposedly you can run larger samples with this method. Even if done correctly and seperation is achieved perfectly, I am stepping away from this path for one reason that wouldn't change, solvent volume. At my scale, it would require more solvent than I am currently willing to work with at this time.

Which brings me toooo......

Tollen's Reagent

I have seen the discussion of selectively oxidizing the leftover aldehyde. I have a friend who is also working on this.

(Feel free to jump in if you want)

I half-assed tried a couple of times earlier on when I was still learning this technique. Nothing that I expected to work nor did the attempts work.

I dismissed the idea of Tollens back then for reasons I don't fully recall but I feel it was having to use silver that turned me off from it. I have always wanted to do the silver mirror experiment. Probably as long ago as I made my first gallium spoon. Fun for the kids (and me).

Ok, enough fluff. I made a solution of distilled ketone contaminated with helional in DCM at about a 1:7 dilution. Put 4 ml (.5 gram ketone) into a beaker and set to stir with a few ml of Tollens. It quickly turned gray, indicating it was working. Let the biphasic mix stir at RT for an hour. Separated, washed with water then brine. A little MgSO4 then TLC. Nadal!

TLC doesn't show a significant decrease in aldehyde. But the Tollens turned dark grey cloudy which should mean it reacted with something. Also, being that this is the main use of Tollens, I know there is a way to make it work.

I think I'm asking if anyone has any suggestions about parameters or reaction conditions? Drip? Heat? PTC? Different solvent?

Any input, feedback or comments are appreciated.

❤️

u/2-5mafia — 6 days ago

Cathinone Amination Solvent?

I'm sure it's due to my weak knowledge of chemistry, but I'm confused on what solvents can be used for the amination of a halo ketone, say 2 bromo propiophenone and similar compounds.

I've seen polar aprotic solvents like ethyl acetate be used, dcm, etc, but then I saw a write up on erowid about using benzene, which iirc is a nonpolar apeotic solvent, during an amination of 2 bromo propiophenone. It was actually the solvent used to bromine propiophenone, and then they threw in some water, methylamine chloride and sodium hydroxide.

My questions are "What solvents can be used?" Is the aprotic part the most important? Would a PTC be needed or help yield?"

I was thinking about an otc solvent mix, which is mostly xylene, some ethyl benzene, and dash of cumene iirc.

Just trying to figure out what can be used.

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u/Ok-Fee293 — 5 days ago

Very Basic Questions Regarding LSD Route & In General

Thanks to Hamilton Morris, I found a very useful book about psychedelic chemistry. Literally "Psychedelic Chemistry" is the name.

In it there was mention of a route which I havent heard of before, where methansulfonic acid anhydride in DMF was used to form the amide.

My quick googling has said it is a bit nasty, but not terrible, just be very safe, fume hood, and all the standard safety procedures and all is well.

My questions on this are "why isnt this more discussed? Am I missing something about the dangers of this chemical? How much of the iso product is formed from this route?"

I am not anywhere near completing this procedure, and if I did, would likely use an amide coupling agent like PyBOP, but this route intrigued me.

Another basic question is related to the hydrolysis step. It was stated in the book that the "ines" ergotamine, ergometrine, etc, can all be hydrolysed using the same procedure. Is there anything more than calculating the appropriate molar equivalent to ergotmaine if you have other compounds that are mentioned that fall under the "ine" category?

Also, can anyone recommend resources to learn more about chromatography in relation to LSD? I just dont understand how one might do chromatography if they only have a precursor compound, and then the product. Ive seen recommended using chloroform and methanol to do chromatography. I understand the bare basics of chromatography, but am really uncertain about anybody the finer points. Youtube videos are helpful, but I just cant seem to wrap my mind around knowing what portions to isolate and keep.

Thank you!

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u/ballskindrapes — 7 days ago
▲ 59 r/TheeHive+1 crossposts

EU controls amphetamine (P2NP) and x-MMC drug precursors following first EU Drugs Agency assessments

https://www.euda.europa.eu/news/2026/eu-controls-nine-drug-precursors-following-first-euda-assessments_en

The European Commission has taken a major step to introduce EU-wide controls on nine high-risk precursor chemicals used in illicit drug production via new legislation published this week. The Delegated Regulation (EU) 2026/314 (1) builds on the findings of the first EU-level precursor assessments carried out by the European Union Drugs Agency (EUDA) in 2025 (see news item).

Eight of the precursors in question are linked to the production of four synthetic cathinones (3-CMC, 3-MMC, 4-CMC, 4-MMC), while one substance (phenyl-2-nitropropene) is used in amphetamine production.

The nine newly controlled substances are:

  • Phenyl-2-nitropropene (for amphetamine)
  • 2-bromo-4′-chloropropiophenone (for 4-CMC)
  • 4′-chloropropiophenone (for 4-CMC)
  • 2-bromo-3′-methylpropiophenone (for 3-MMC)
  • 3′-methylpropiophenone (for 3-MMC)
  • 2-bromo-4′-methylpropiophenone (for mephedrone / 4-MMC)
  • 4′-methylpropiophenone (for mephedrone / 4-MMC)
  • 2-bromo-3′-chloropropiophenone (for 3-CMC)
  • 3′-chloropropiophenone (for 3-CMC)

The regulation will apply from 18 September 2026, with a four-month transition period for industry to adapt to the new requirements. It comes as illicit drug production continues to expand within the EU, particularly of synthetic stimulants such as amphetamine, methamphetamine, MDMA and synthetic cathinones. In 2023, 53 synthetic cathinone production sites, some of which were large-scale, were dismantled in the EU, with the majority located in Poland.

The EUDA’s expanded competence in the area of drug precursors entered into force in July 2024. Under the EUDA regulation (Article 14), the agency supports the European Commission and Member States by monitoring precursors used in the production of both controlled illicit drugs and new psychoactive substances (NPS).

Precursor assessments provide evidence on how these chemicals are used, trafficked and distributed and explore the potential impact of chemical, pharmaceutical and research sectors. They are intended to support a consistent EU‑wide understanding of precursor‑related risks and to provide a scientific basis for regulatory and policy decisions at EU level, particularly in relation to scheduling and control measures.

Drug precursors are substances essential to the manufacture of synthetic drugs such as amphetamine, methamphetamine, MDMA and synthetic cathinones, and to the processing of cocaine and heroin. Effective regulation of these chemicals that may be exploited for illicit drug manufacture is essential for early detection of emerging risks and for preventing the diversion of these substances into illicit supply chains.

Notes

^(Regulation EU 2026/314, which will apply as of 18 September 2026, amends the existing drug precursors framework under Regulations EC No. 273/2004 on the internal trade of drug precursors, and No 111/2005 on the trade between the Union and third countries. The European Commission has provided a 4-month transition period for economic operators to adapt to the new requirements. At the same time, the Commission continues the work on a broader revision of the EU’s precursor control framework. The draft proposal on monitoring and controlling drug precursors was published at the end of 2025. With this new regulation, the Commission aims to respond to shortcomings identified in the existing framework, including difficulties in addressing rapidly emerging “designer precursors” and inconsistencies in enforcement across Member States. It aims to strike a balance between preventing diversion into illicit drug production and preserving the legitimate industrial and commercial use of chemicals.)

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u/Borax — 9 days ago

Bioisosteric Methylone analogs - βk-ODMA, βk-TDMA, and βk-SeDMA

There is a relatively new study(2024 https://onlinelibrary.wiley.com/doi/10.1111/jnc.16149 ) that investigated bioisosteric analogues of MDMA, specifically ODMA, TMDA and SEDMA, since it is not a phenyl ring, it does not fall under the classic blanket bans that very extensively structurally regulate amphetamines and cathinones.

One research chemicals lab was inspired by that work and created something functionally like pyrovalerone with that bioisosteric modification (ODPV)

but I think it will probably be too strong, "pyros" are generally very feared among people who do not consider themselves crack heads. my favorite substance is 2MMC (oral ROA) "reasonable" but intense dopamine rush and it softens and smooths the edges a bit with that slight serotonin effect - for me perfectly balanced, I'm not a fan of pure empathogens with a high preference for serotonin transporters over dopamine (I don't prefer MDMA, 6APB, 5MABP) but I also avoid pyrovalerenons, that's why I like 3MMC and 2MMC, because it's a real stimulant, addictively similar to cocaine - so it's not really vegan, it's dope but it's not pyro or similar madness, and it has what we love about cocaine and amphetamine and at the same time a bit of what we love about sero-empathogens, this profile suits me the most.

BK-MDMA, so methylone is still an empathogen, although it no longer has such an extreme preference for serotonin transporters over dopaminergic ones like mdma , but there is still a significant preference so I still classify it as a primary serotonin empathogen, even though it is a cathinone, I do not classify it as MMCs, but I still classify methylone more as MDMA and benzofurans (6APB..) even though the BK group makes a difference towards what I like, but it still does not have the preferred dopaminergic drive for me like MMCs have.

Based on studies of bioisosteric analogues of MDMA, it seems that some ring modifications (I think SEDMA and tdma) will significantly increase the preference for dopamine transporters over serotonin transporters - and when we know that the BK (cathinone version) group also increases the preference towards dopamine in the case of methylone (bk-mdma), it occurred to me that very theoretically, the bioisostere of methylone bk-tdma bk-sedma could shift the profile even more towards dopamine and approach or reach the level of MMCs (methylmethcathinones) - of course it was done only on cells and of course preference is not everything and does not speak 100% about absolute values ​​and the entire dynamics of the effect on monoamines, etc., etc., but it gives a decent theoretical basis

that it is supposedly difficult to synthesize, at least to discover a chemical route to stably synthesize it, I don't know much about synthesis, could any of you do it?

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u/Ok-Landscape-7087 — 11 days ago

I noticed a substance on the NPS market that is supposed to be bioster MDPV, according to them, so that it does not fall under the blanket ban in NL, from the chemical structure in 2D view it looks for non-chemist(me) like one double bond in the aromatic ring is missing and there is an attached structure that resembles MD, but it contains oxygen and two nitrogens with double bonds, see CX717 on wiki, same core

very interesting, what do you think about it?

https://preview.redd.it/k4f9czv21wzg1.png?width=1200&format=png&auto=webp&s=7a26884306a5753499220a5793cab24c663213cc

1-(benzo[c][1,2,5]oxadiazol-5-yl)-2-(pyrrolidin-1-yl)pentan-1-one'

Pyrrolidine was chosen for the alpha position and there's an ethyl is on the terminal amine, similar to what we know from N-ethyl-pentedrone, interesting, if that's all true then it's going to be big.

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u/Ok-Landscape-7087 — 14 days ago