Sciencemadness Discussion Board

Have any of the sciencemadness members discovered anything?

100PercentChemistry - 23-7-2017 at 17:19

Has any user discovered anything( big or small) in their home lab? If so what was it?

JJay - 23-7-2017 at 17:36

I discovered something but I'm afraid that I'll be denounced as a heretic or burned at the stake if I reveal it :)

clearly_not_atara - 23-7-2017 at 18:12

Ullmann's methyl ethanesulfonate synthesis used two known reactions but put them together in a way that hadn't been done before:

https://www.sciencemadness.org/talk/viewthread.php?tid=9921&...

j_sum1 - 23-7-2017 at 18:24

blogfast25 developed some novel thermite reactions for Ti and Si and included some booster reactions involving calcium sulfate.
I believe that the Hofmann degradation to form hydrazine was refined on this board. Take a look at some older YT clips and compare them with some newer ones to see what I mean.
Dan Vizine devised some original methods for isolating thorium.
Take a scan down the list of prepub and you will find some more (and possibly better) candidates.

symboom - 23-7-2017 at 19:49

I dont know if it is new or hard to find but Chemetix had a method for nitric acid quite an acomplishment of Ostwald style nitric production but without platnium not sure if it has been done before

I have none my main projects are energetic complex salts and inorganic peroxide salts nothing new im more replicating it in an amateur chemistry setting.

Performing experiments that are normally designed for industry
Or profesional laboratories with lots of equipment but done in a home lab such as
ethyl perchlorate or LLs copper hexamine perchlorate or hydrazine and azides

Or making sodium or ceasium metal many labs dont even make that they just buy many of the things

Im sure there are a few in the organic chemistry side who have come up with some others

[Edited on 24-7-2017 by symboom]

j_sum1 - 23-7-2017 at 20:03

Forgot about Chemetix. As I recall he is still working on that project but it looks really promising.

And don't forget Len1. He tried out many of his procedures while active on this board. His book on small scale syntheses is a classic. Few of his synths are completely original but they have been adapted / simplified to make them accessible to do in non-industrial volumes. IMO this qualifies as "discovered something".

Cou - 23-7-2017 at 21:57

Quote: Originally posted by 100PercentChemistry  
Has any user discovered anything( big or small) in their home lab? If so what was it?


who says a discovery has to be something earth-shattering that affects the studies of every scientist in the world?

take a look at the prepublications forum... amateur chemists have developed helpful procedures that help other amateur chemists, and that is science/innovation

brubei - 24-7-2017 at 03:10

from wich impact factor publication can we tell we did a discovery :D ?

ave369 - 24-7-2017 at 03:22

I discovered some procedures that are specific to home chemistry and are pretty useless in a professional lab, such as a novel way to prepare concentrated sulfuric acid from battery acid without a fume hood.

Metacelsus - 24-7-2017 at 04:08

I've discovered some stuff (syntheses and properties of new compounds, for example) but I did the work in a university research lab, not in a home lab.

karlos³ - 24-7-2017 at 06:11

Do chemicals unreported in the literature, even slight variations of known compounds, count as discovery too? Even if its, for example, a designer drug?

tsathoggua1 - 24-7-2017 at 09:16

What about Nurdrage? and both his synthesis/purification of 1,4-dioxane from antifreeze and drain cleaner grade sulfuric, with the crap in them not carrying over during distillation of the dioxane; and then his subsequent employment of the dioxane to purify the MgO/metal composite, prepared by thermite-ing alkali metal hydroxides with Mg dust, taking the result from something that starts out looking like cement, and after subjecting it to grinding in a blender (inert gas here doubtless would improve the yields) boiling the aggregate once powdered in 1,4-dioxane to get, for example, dirty great lumps of fresh, clean sodium metal. Making a valuable resource to hobbyists, although most commercial labs would just buy it, many hobbyists cannot, and in the past resorted to finicky electrolysis requiring much work and design into a process a 10-year-old kid could do with youtube and enough money for antifreeze, magnesium, caustic soda, some sulfuric drain cleaner and some very basic glassware/hotplate (I.e a conical flask and a bit of coat-hanger wire to poke about in there plus as many soup cans as desired and some slabs of stone etc. to stick over the top and prevent the alkali metals from vaporizing off.

That has to be one of the finest hours of our mad scientist community. Effectively making sodium, potassium, rubidium, caesium more or less OTC (albeit through ebay in the latter two cases to obtain the hydroxides or salts to prepare them from) and slashing the effort needed to get from compound to element from reasonably intricate and needing a lot of time put in to cell design for electrolytic routes to 'add A to B, distill, purify' and add C to D, put in soup can or equivalent, light the bugger, cap it and step back, remove result, powder it and boil in the result from step 1'

I'd say that is pretty damned impressive a piece of innovation, and one that makes both a useful, previously for some of us, difficult or impossible to buy, plus the scores of useful reagents even more difficult to buy (fr,ex the hydrides and borohydrides, plus Na-based Birch reductions, and Boveault-Blanc reductions using Na/anhydrous EtOH. Na/anhydrous NH3 in the form of small pellets or prills of Na, in anhydrous diethyl or diisopropyl ether with a continuous stream of anhydrous ammonia gas (have always done this using ice/salt/methylated spirits/CaCl2/HCl solution to cool it externally, but have been told apparently the solvated electron solution forms more rapidly when done at RT than cold but have not yet tried an RT birch. This is NOT akin to 'shake 'n bake' meth cooking where such cooks use pressurized bottles and 'burp' them to release the pressure hoping to god and satan both that it doesn't blow their balls off first but rather uses continual stream of NH3 and finely divided Na, or else battery lithium, which works well due to the very large surface area of the thin Li foil, when cut to pieces, and stirred vigorously, using an aquaculture-style airstone diffuser to introduce the gaseous anhydrous NH3 under an argon atmosphere. Takes a while to generate the Li or Na-blue but it does work and saves on having to mess around with liquid anhydrous ammonia. One just has to add the substrate as a slurry in an alcohol to serve as a proton source, the NH3 excess being led both in and out through a drying tube, using a 2-neck or 3-necked flask.

And the NH3 being generated using CaO as a base with an ammonium salt such as the sulfate or phosphate, the CaO serving both to dessicate the NH3(g) and not producing water as a byproduct as would happen when hydroxides are used as the base.

https://en.wikipedia.org/wiki/Bouveault%E2%80%93Blanc_reduct...)

Alkali metals relatively cheaply and much easier than electrolysis.

tsathoggua1 - 24-7-2017 at 09:25

Also, soon as Tsath' gets some more nitromethane and nitroethane he will be getting to finish up on his 3-bromo-4-(1,1-difluoromethoxy)-5-methoxyphenethylamine project along with the alpha-methylated homolog of the same. As far as thus far he can find this has never been synthesized (although he is part way through reading the Shulgin index and may yet find it of course) and reducing the intermediate nitroalkenes with Red-Al (expensive, but so was the intermediate aldehyde, £90-something for 5g so the mildest of routes must be used and the cleanest reduction methods, especially since he got lucky with that aldehyde, and may never be able to obtain more)

IF he can get more of the benzaldehyde he'll also go for the pthalimidopropiophenone too, to serve as an in-vivo prodrug protected cathinone homolog, to avoid the issue of primary beta-ketoamines dimerizing to pyrazines. The idea being to cleave off the pthalimide in HCl, but rather than in a flask, risking dimerization in a conc. solution, keep it stabilized as the phthalimidopropiophenone, and rely on gastric acid to perform the hydrolysis, keeping the solution dilute and thus doing as much as possible to keep the molecules of the liberated cathinone from bumping into each other and dimerizing prior to systemic absorption.

This isn't a 'street drug' distribution effort or anything, but rather, out of genuine interest, there seems to be next to NOTHING involving phenethylamines, amphetamines, aephetamines or cathinones/alpha-ethyl-beta-keto phenethylamines in the published literature with electronegative substituents on the 3- or 4- position, especially in the case of groups that withdraw electron density from the phenyl ring on the 3' phenyl carbon.

Can't do it JUST yet, since he is almost out of nitroethane and utterly out of NM. He needs what nitroethane he has left, to prepare some pure mono-ethylamine (via acid/Fe reduction and distillation into HCl and he is down to maybe 60-70 to 100ml or so of NE)

[Edited on 24-7-2017 by tsathoggua1]

Texium - 24-7-2017 at 15:42

Quote: Originally posted by tsathoggua1  
Also, soon as Tsath' gets some more nitromethane and nitroethane he will be getting to finish up on his 3-bromo-4-(1,1-difluoromethoxy)-5-methoxyphenethylamine project along with the alpha-methylated homolog of the same. As far as thus far he can find this has never been synthesized (although he is part way through reading the Shulgin index and may yet find it of course) and reducing the intermediate nitroalkenes with Red-Al (expensive, but so was the intermediate aldehyde, £90-something for 5g so the mildest of routes must be used and the cleanest reduction methods, especially since he got lucky with that aldehyde, and may never be able to obtain more)

IF he can get more of the benzaldehyde he'll also go for the pthalimidopropiophenone too, to serve as an in-vivo prodrug protected cathinone homolog, to avoid the issue of primary beta-ketoamines dimerizing to pyrazines. The idea being to cleave off the pthalimide in HCl, but rather than in a flask, risking dimerization in a conc. solution, keep it stabilized as the phthalimidopropiophenone, and rely on gastric acid to perform the hydrolysis, keeping the solution dilute and thus doing as much as possible to keep the molecules of the liberated cathinone from bumping into each other and dimerizing prior to systemic absorption.

This isn't a 'street drug' distribution effort or anything, but rather, out of genuine interest, there seems to be next to NOTHING involving phenethylamines, amphetamines, aephetamines or cathinones/alpha-ethyl-beta-keto phenethylamines in the published literature with electronegative substituents on the 3- or 4- position, especially in the case of groups that withdraw electron density from the phenyl ring on the 3' phenyl carbon.

Can't do it JUST yet, since he is almost out of nitroethane and utterly out of NM. He needs what nitroethane he has left, to prepare some pure mono-ethylamine (via acid/Fe reduction and distillation into HCl and he is down to maybe 60-70 to 100ml or so of NE)
Can you keep your psychotic sounding 3rd-person cookery drivel to yourself please? Take it to a drugs forum or something.

JJay - 24-7-2017 at 17:39

Quote:
This isn't a 'street drug' distribution effort or anything, but rather, out of genuine interest, there seems to be next to NOTHING involving phenethylamines, amphetamines, aephetamines or cathinones/alpha-ethyl-beta-keto phenethylamines in the published literature with electronegative substituents on the 3- or 4- position, especially in the case of groups that withdraw electron density from the phenyl ring on the 3' phenyl carbon.


You should probably be aware that 4-chloroamphetamine is used in research as a neurotoxin that selectively kills serotonergic neurons. 4-ethylamphetamine has some kind of really nasty side effects too IIRC. You really should take drug discussion to drugs forums, ESPECIALLY if you are considering human trials of a novel designer drug that has never been tested on animals (which in my mind is unethical because it might kill or seriously harm humans needlessly). In any event, most amateurs do not have labs that are suited to producing psychoactive substances of sufficient purity and in forms that are suitable for human consumption. Even drinking distilled water that you make in your lab is frowned upon.

If you are hellbent on testing on designer drugs on people, though, please do post your findings. But not here.



[Edited on 25-7-2017 by JJay]

j_sum1 - 24-7-2017 at 18:51

Quote: Originally posted by tsathoggua1  
What about Nurdrage? and both his synthesis/purification of 1,4-dioxane from antifreeze and drain cleaner grade sulfuric, with the crap in them not carrying over during distillation of the dioxane; etc...

Agreed. Revolutionary stuff by an amateur chemist. But he hasn't been a member of these boards for some time.

tsathoggua1 - 25-7-2017 at 13:27

Well to me, animal testing is extremely unethical especially for that kind of project. They can't consent. I can. I'm not about to start testing things on unconsenting anybody.

And I don't do animal research, that is one line I just will not cross. I understand why its done in medicine. But I don't have to like it, and I sure as hell don't have to stain my hands with animal suffering and misery.

Also, I think, aside from some known behavioural reactions to things like 5HT2a agonists, and other serotonergics, NMDA antagonists, opioids, sedatives, psychostimulants etc. the nuances of psychedelic chemistry are completely unfathomable through animal testing to begin with. A rat can't tell you what its thinking, and it sure isn't going to know what the hades just hit it. It'll just get confused, and probably feel pretty sorry for itself. It takes the higher cortical functioning of a reasoning, self-aware mind capable of existential thought and self-reference to process such things in the first place.

And although thanks, I am aware of the toxicity of para-substituted amphetamines in general (fluoro aside, at least as a serotonergic neurotoxin) as well as catechol type substitution patterns.

This does seem limited however to para-monosubstitution. None of them (perhaps 4-FA aside, although I haven't personally bioassayed it. seem to have much good to be said about them. And 4-methyl, 4-MeO-amphetamine are downright notorious. PMA certainly is, and according to my reading para-CH3 causes some pretty significant 5HT depletion and long lasting negative effects.

4-methylthioamphetamine perhaps would have been different, maybe, if it were not for the MAO-a inhibiting properties it exhibits. and 3-monosubstitution with a highly electronegative substituent isn't well known. Fenfluramine is the only main one I can think of, aside from 3-fluoroamphetamine. And that has the major issue of both long duration of the parent drug and also the metabolite, norfenfluramine. Both being significantly potent 5HT2b receptor agonists, which presents the danger of cardiac valvulopathy. Perhaps usually with chronic use, such as with fenfluramine as a diet drug historically speaking, but it is very long acting, and its metabolite is just as potent or more so as an 5HT2bR agonist.

Its a different matter entirely with 2,5-alkoxy/alkylthio or 3,4,5-alkoxy, alkylthio substitution, vis a vis mescaline and TMA, along with the TMA positional isomers. Difluoromescaline is a known entity and active in humans, that much is known,as well as some degree of knowledge of in-vivo potency in humans. DOI, DOB, DOC don't share the serotonergic neuron ablative properties of the corresponding para-monohaloamphetamines, or we'd have definitely known about it by now, especially given the likes of studying DOI as a TNF-alpha inhibitor (quite a potent one too by all accounts).

I'm not just doing this to turn a quick buck. I am genuinely interested in the pharmacology of this hitherto, as best as can be determined, unknown derivative.

Don't take at face value and just tar me with the 'another bloody meth cooking redneck hick' brush. And I fail to see what is psychotic about wishing to explore new ground. There is no reason to resort to insult. I have not.

And you know something, its a damned shame that intelligent people such as are here, are taken in by decades of propaganda, in part fuelled by racism (vis a vis reefer madness, and cocaine,) and in part by industry pressure, with a generous helping of ridiculous BS. 'all drugs are bad' without considering what one is, or does, unless prescribed by a doctor, developed by a pharmaceutical company et cetera, whilst prohibiting organized 'legitimate' study of these compounds and the potential benefits they can with the right applications in the right circumstances, bring.

Entactogens, for example (AMT) helped me with PTSD.

j_sum1 - 25-7-2017 at 14:42

Quote: Originally posted by tsathoggua1  
Well to me, ani... etc etc etc

Way off topic again Tsath.
There are so many issues with the content of your post, but ultimately they don't belong here and probably not on this board.

clearly_not_atara - 25-7-2017 at 15:26

Tsath, I understand from previous conversations elsewhere that you've been having some "issues". First of all I suggest you avoid defending yourself as you are likely to do so poorly.

I suggest you relax, take some time off of the Internet, and do not use more than maintenance levels of drugs.

Quote:
And you know something, its a damned shame that intelligent people such as are here, are taken in by decades of propaganda, in part fuelled by racism (vis a vis reefer madness, and cocaine,) and in part by industry pressure, with a generous helping of ridiculous BS. 'all drugs are bad' without considering what one is, or does, unless prescribed by a doctor, developed by a pharmaceutical company et cetera, whilst prohibiting organized 'legitimate' study of these compounds and the potential benefits they can with the right applications in the right circumstances, bring.


It is certainly not the case that all drugs are bad, but unknown drugs are likely to be bad, so fervent experimentation with novel compounds, and particularly those which are not close analogues of well-known compounds, is nearly certain to incur bad effects. For this reason it would not be wise to do so if your mental state is already problematic. Such as now.

Everyone else, please be nice. Toady has experienced more of the negative side of drug use first hand than you are likely to be able to scare him of with words.

[Edited on 26-7-2017 by clearly_not_atara]

tsathoggua1 - 26-7-2017 at 15:20

I was replying (regarding animal testing) to JJay, who had suggested that going from in synthesis, in vitro directly to humans was (potentially) immoral. So it isn't really off topic to take the time briefly to respond to that concern.

And is the point made about animals lacking in higher cortical functions such as present in us, the great apes, probaly cetaceans and elephant (and not that I happen of course to keep such 'around', nor would I, for precisely those reasons) in this particular field of study then whatever we could learn from animals like the humble lab rat, is more or less made obsolete, what we can learn in tissue culture should be sufficient for neurotoxicity studies and receptor binding/ligand displacement assays. So there is no need, or indeed good that can come from subjecting a whole (arguably), living creature capable of suffering to the compounds in question, cytotoxicity of course is something that should be ruled out, as is (potent, significant) irreversible inhibition of MAO-a, as well as any potential for covalent receptor binding with the aryl bromide.

Apologies for the perhaps quickly drawn up post, at the time it was made, I was in a hurry to get the main points down, with a few minutes of computer access left and somebody standing over me wanting to use the computer.

not_atara, just a couple of points, I haven't been 'fervently' experimenting with many what you could call novel compounds, not novel as this. A few trial doses of various obscure opioids at times, occasionally, mostly (not got much, being on pain medication chronically, to lose from dependency risk, and any trials are not done for so long as to risk intensifying what already exists)

All I'd be calling for, is reasoned and civil discusssion of the results, when finished, if permissible. And also for theoretical discussion on the biology of phenethylamine/alpha-alkylphenethylamines bearing the 3,4,5-substitution pattern and having as opposed to the electron-donating nature of the methoxy group found in nature's template for this substitution pattern, mescaline. I don't see how wishing to know of existing research in this direction is a bad thing, and given such a project in development, not the most responsible way to go about initiating the project in question. It makes sense to do the background research as thoroughly as possible, and quite the opposite to do otherwise.

not_atara-btw this isn't exactly that distant an analog of a known compound. The homolog of mescaline bearing a difluoromethoxy moiety in place of methoxy, is already known and has I believe been tested in man, with an active level found at

(will have to finish this tomorrow, no time)

j_sum1 - 26-7-2017 at 16:28

Ok. But the OP is "Have any SM members discovered anything?"
To that end, a lot of what you have posted is off topic -- it deserves its own thread. Why don't you start one and ask for the mods to prune this one?

symboom - 26-7-2017 at 17:30

Karlos I dont see why not
Even slight change in the compound it may have entirely different properties

j_sum1 agreed this is getting way off topic
tsathoggua1 im reading your first post and im confused your first post was half relevent than is takes a large dive into the abyss was trying to atleast see if there is any discoveries if you truly feel that way I suggest a concise write up showing exactly the chemistry just like any researcher would do with any drug if he wasnt so consumed with psychedelics he might be able to help in the organic chemistry forum and expand amateur organic chemistry
My unbiased view hopefully

Bouveault–Blanc reduction probally the most interesting thing I read about

tsathoggua1 you could always just post the chemical name
Im sorry JJay I added the wrong user name

To save time from the rambling hes working on synthsis of
3-bromo-4-(1,1-difluoromethoxy)-5-methoxyphenethylamine project along with the alpha-methylated homolog

I think hes also trying to make this
para-substituted amphetamines
Difluoromescaline
4-methylthioamphetamine
Hopefully this helps as a translation
I dont know organic chemistry well so I could be wrong
I know my post is after the other posts and my post might also end up in deletruis this is off topic anyways

[Edited on 27-7-2017 by symboom]

[Edited on 27-7-2017 by symboom]

JJay - 26-7-2017 at 18:21

@symboom: Your post as currently worded states that I'm making designer amphetamines. This assertion is both false and utterly without merit, and I would appreciate it if you would not libel me in this manner.

symboom - 26-7-2017 at 18:57

I appologize JJay I ment to say tsathoggua1 and the place ment of your username ahead of that statment did not help that.
And then I was going to say JJay I dont wont to feel like im encouraging tsathoggua1.
Now I remember why I dont get involved in these types of discussions.

[Edited on 27-7-2017 by symboom]

Melgar - 27-7-2017 at 04:19

I discovered that certain types of free radical chlorination reactions can proceed much faster and with much better selectivity by adding a catalytic amount of bromine. Since bromide salts will release bromine in the presence of chlorine, bromine can be added via a bromide salt or organobromide, if chlorine or TCCA is already present.

I also discovered that ETN will detonate via thermal shock in the presence of aluminum.