DMT and other tryptamine synth questions….please help…

[Rabidreject]

Okay so I have two syntheses of n,n-DMT and a rough idea of a synth for DET also.
I have a couple of questions that I really need answering. I am not going to list the steps or anything, just the general gist of what happens in them or how they differ and why that confuses me.
I have done the MHRB extraction - many times before and it’s what got me interested in organic chemistry as a hobby.
I am aware of two syntheses for turning tryptamine freebase into n,n-DMT and potentially DET, with just a slight tweak.
Okay so, I call the two different methods the hamiltons crazy three eye balaclava guy’s synth or a Reddit synth.
I have seen links to both of these on this forum so it’s not like I’m coming up with anything new but I’m concerned about the Hamilton’s mad guys route due to hearing mumbles about him saying they actually did something different to the synthesis he gives but honestly it looks fine to me - the thing I don’t really understand is that at the end of Hamilton’s video he says - “after the rxn mixture has sat to completion, you use PH manipulation anagolous to when you do it from plant matter.
So seeing as it utilises STAB, made in situ just before running the rxn, instead of standard NaBH4, it is going to already be acidic I would imagine (due to using glacial acetic acid to make the STAB) but if not - do I literally use the exact same things for the acids and alkali’s one would use in a MHRB extraction (5% white vinegar + NaOH)?
Secondly, I am assuming you wouldn’t extract it using naptha, due to it being a low quality petroleum product, as opposed to something like chloroform or DCM? I also have access to diethyl-ether but I’m not sure if it’s the correct polarity. Oh yeh one more question about this synthesis is why do they need to use PH manipulation to ‘extract’ the DMT from this RM and yet they don’t say to do that in the second synthesis? - it seems like this synth makes it easier to x’stalise than the second one.
I have DEFINITELY heard of people crystallising from boiling hexane, as is mentioned in the second synth I found.

Okay so for this one - yes, I know it came from Reddit and isn’t the best source - I say that like most of Reddit stuff is realistic and likely to work, which when you delve into this subject some things seem to have been written by people who actually understand the subject and others just write bullshit. This one seems okay and isn’t SO different to the first, it all has to be carried out at <= 0 degrees c - same as the other.
It also utilises a lot of the same reagents; tryptamine, formaldehyde and sodium borohydride being the three standard molecules iv seen people use to make tertiary tryptamines.
The difference being, I am assuming that NaBH4 isn’t as ‘strong’ of a reducer as STAB, because you have to do two seperate reductions, adding more boro to take it from NMT to DMT in the second synth. He also doesn’t use PH manipulation to try to crystalise it and instead cleans it up first as an oil and then he /she crystalises from boiling hexane.
I guess it’s hard for people to chime in if they’ve not seen either synth so here is a link to the Hamilton one (I went to settings in pootube and slowed it down to half speed, I believe) Hamiltons way.
Then you need a link to the second synthesis of it which is here: Mr Reddit’s Way.
I am really hoping you can help me to be honest as I’m a little flummoxed….
Oh and also - iv seen that if you substitute the formaldehyde for acetaldehyde that it would essentially form DET…although I’m pretty sure he just wrote to use NaBH4 for that - he also uses just NaBH4 for his 5-meo-DMT synthesis as well which leads me to think this is his preferred chem to use over STAB but then again, the crazy chemist says stab is better for carbonyl’s.
I’m not short on tryptamine AT ALL, seeing as you are pretty much forced into buying en-mass from China - or decarb it yourself from tryptophan but that’s a horrible rxn to do and it is better run in an inert atmosphere or under vacuum to bring down the boiling point. Anyway I abandoned that project - it’s not an ideal first rxn to complete!
The thing I like about the second RXN method is it doesn’t use up my VERY limited supply of DCE and glacial acetic acid. Obviously tryptamine is fairly heavy as a molecule and therefore it means you end up using more solvents and acids - or I guess I should say, it utilises harder to obtain solvents and acids than the second method.
I think I plan on trying the second method first to be honest. I may well take a trip back to rhodium and see what the synths are saying on there as iv not checked there in a while - certainly not since iv had tryptamine.

If someone is able to clear up literally ANY of these questions I’d be incredibly grateful. I’m awaiting getting paid tomorrow to be able to buy more anhydrous methanol and will most likely buy some dry ice (I have plenty of acetone) which should keep it nice and cold.

It just makes sense to me that you would alter the PH in order to manipulate the product, clean it up a little and allow it to x’stalise. Then re-x….and probably re-x again given that I’ll most likely be doing either subcutaneous injections or if I can get a drip machine / medicinal infusion machine, I can ride the waves and explore the DMT-scape a little better and maybe be able to remember a little more….

Also, I know there is a lot in this post - if you have performed this RXN personally could you possibly chime in and let me know which method you went about it in? I am not looking to milk the cash cow here - this is literally for my learning as well as maybe my own personal use. I heard yesterday on hamiltons podcast there is a company in Spain that will test alkaloid content of organic matter as well as doing GCMS on whatever sample you send in….pretty exciting stuff - probably WAY outside my budget but we’ll see!
It’s funny how tryptamine smells like DMT. That sort of plasticky type smell - I’m not willing to see if it tastes the same when inhaled though!!
On a more serious note - although I may not get it tested professionally, I will be doing TLC to make sure the RXN is complete - trouble is my glass plates are MASSIVE. Could I get a glass cutter and cut the silicon sprayed plates from 20cmx10cm to 10cmx5cm. Then i would have 5 much smaller plates that will actually fit into a beaker I own instead of having to buy a huge beaker to do any TLC…
Also; watching hamiltons 5-meo-DMT synthesis that he does in Mexico; I noticed he used paper TLC for the same reason and his pieces of paper are about the same size I would score and knock the glass off as. I’m just wondering how he can get away with using paper for TLC when everyone else I have spoken to says that you should be using glass plates sprayed with silicon - I just didn’t look at the size! I have a black light for said usage but if I can get away with using some sort of paper TLC that’s going to be easier.
Thanks in advance - sorry this post is a bit is a scatter of chaos!
Hope you can help with at least something!
RR

 

[Rabidreject]

Sorry, one more thing, I have a shit ton of the stuff (tryptamine) that It made financial sense to buy - seeing as most places selling less were a similar price.
I’m also a keen photographer/cinematographer and therefore once I get the synth correct am more than happy to do video’s of the DMT and also the DET synthesis, if it would help people in the future.

 

[Rabidreject]

Okay - forget about the TLC questions. I just found this great article that answers my questions re-TLC testing - https://www.critical.consulting/post/low-tech-method-for-tryptamine-analysis

 

[mescalito10]

"Mr. Reddit", is she, Norolinda. Just do it exactly as she did and you will succeed. Maybe you can wait shorter between addition, repeat immediately when when the temperature drops enough. I don't know how low is enough. 0C or slightly below should be ok, you can try -5C or -10C and report your yields. You can also do 6 or 8 additions insted of 4, but with smaller amounts, so the same total but in more parts. But even if you don't change anything it's an okay procedure.

 

[Rabidreject]

Ah that’s awesome! Finally someone who has actually done the synth first hand!
It’s either hard for me to find specific info because it’s the way in which they earn their living and so TOTALLY AGAINST the spirit of chemistry, sit on their knowledge and will only part with it for cash or if you REALLY know them.
Can I ask where, generally, people find their syntheses because shamefully it usually comes down to (unless it is on this website somewhere) YouTube, patents or just plain google searches and fumbling about there….usually to no great success. Oh or Reddit! I do try to see if multiple people are using the same method (on YouTube for example I’ll make sure a few people are doing the same thing - like recently I had to make sodium ethyl sulfate and there was a great video on there but I had to just tripple check multiple people are using it.
Cool, okay, I’ll work out my quantities (in g) from said DMT synth and get to work…I’ll have to substitute the water bath for a mantle (it’s one with a PTFE protected temp probe) and the rotovap with distillation - probably under as much of a vacuum as I can muster from an aspirator I’m about to buy. Oh and dry ice and hexane - I’m hoping hexane is relatively easy to buy here
I assume this will be okay only more work? I mean, I guess I could make a water bath but it would just be a pot of water on the hotplate lol this response is far too long sorry! I shall report my findings, no doubt I’ll fuck it up a time or two but hopefully not - i am in the middle of writing it down and writing my notes, simplifying the writing and putting into steps as much as possible. I’m glad it works though - have you ever tried the former method?

 

[Rabidreject]

Oh okay, I just bought a water bath coz it was super cheap from China. It just means I can pop it in and forget - yup, I’m lazy!

 

[mescalito10]

No, I haven't tried the STAB route, as supposedly it doesn't work with mexamine.

Some people have preffered cyanoborohydride like this guy: https: //www.thevespiary.org/talk/index.php?topic=15189

Here's the best DMT thread at The Vespiary: https://www.thevespiary.org/talk/index.php?topic=16470.0

Here's details of the Hamilton's Synthesis: https://1lib.sk/book/18611424/2746f...lic-toad-of-the-sonoran-desert-synthesis.html

There's also some tryptamine chemistry also at the russian website Hyperlab.

You don't need rotovap, simple distillation is enough. You don't need vaccum. You don't need dry ice, normal crushed ice and salt water dripped over it will do. You don't need hexane, actually you don't want hexane, it's neurotoxic in a way that for example heptane isn't. You can use heptane, hexane or any mix of them in any proportions. Optionally with the addition of diethyl ether, 1:9.

I would like to help you more, but you write a lot and I am not sure what exactly you are asking about.

What kind of water bath did you buy and why?

 

[Rabidreject]

Oh that’s fine, I have diethyl-ether anyway so that’s great, iv been waiting for a use for it lol

 

[Rabidreject]

Just a simple water bath with timer and PID heated. It was $40 so I figured why not - it isn’t necessarily for this. I will have tried it a few times by the time that arrives, I’m aware of that. I also bought a vacuum aspirator while I was at it and some more boro stirring sticks - fuck I always sound so unprofessional as I can’t remember what simple things are called. I had a mind blank earlier as I needed a beaker and kept searching for different flasks! Took me ages to realise it was, of course, a beaker. Just getting mind blanks as i am coming off a twenty year benzo habit. So my heads fucked and the whole reason I had to confidence to start this VERY expensive endeavour as I don’t JUST want to make DMT. In fact I actually want to focus on phenethylamines but at the moment I don’t have a link for the nitromethane and nitromethane I need.
can the former be separated from that RC fuel? Some people say yes some no

 

[Rabidreject]

Re-reading this now is quite interesting.
so I have tried the synth. I’v basically ended up with a dark yellow/ish oil and I’m finding it really hard to re-x from using boiling heptane - it just doesn’t mix.
I did it yesterday - although admittedly the oil that I ended up with during the synth has been sat around a week or so because I didn’t have heptane and it took longer to come than expected.

Have you got any advice for the final re-x?

I tried a freeze precip after because It didn’t really say how to re-x from heptane and I noticed it went cloudy when picked up with a cold pipette.
I got shamefully few crystals but it really reminded me the many extractions iv done from MHRB.
I’ll try and add some diethyl-ether and see if I get any better results and if not I’ll have to evap the heptane..

 

[Rabidreject]

It is a possibility I let it get too warm as I stupidly added all the formaldehyde (for each addition) at once and to be fair, I could have slowed the addition of the NaBH4 as well.
I think I shall re-try the synth now that I have everything (annoyingly other than a vacuum dessicator)

 

[mescalito10]

It doesn't get too warm with addition of the formaldehyde. The error is earlier, it's just that you didn't start cool enough. Then also assure you have a very good mixing and add borohydride so that you add in powder of the borohydride and not big clumps/rocks of it. Put it on paper on something and chip at it with a spatula so only powder goes in and the mixing is strong. Only error is not being cold enough before adding formaldehyde. -20C recommended. -10C to -5C is still okay if the amounts are not big. 50% yield guaranteed even with a shitty workup. Be sure to evaporate as much methanol as you can before begining the work up. I also begin to think that ethyl acetate is better for workup than DCM.

 

[mescalito10]

Yellow-orange-reddish oil is good. Yes this shit is hard to disolve, use more heptane and then cool it down, no need to evap.
No problem with adding all the formaldehyde at once. Just do it again, extract immediately using more heptane and you are good I think.

 

[mescalito10]

Because you have been extracting it from reaction mixture using what? DCM? Chloroform? Ethyl Acetate?

 

[mescalito10]

From DCM the oil ends up a little bit Orange after distilling DCM.

 

[buffalophill]

is anyone ready to make a video yet?

 

[buffalophill]

synthesis from https://www.thevespiary.org/talk/index.php?topic=15189.new#new

Hey guys, a couple of people have been curious as to how RP made his synthetic DMT, so here you go. Enjoy!

This is for a 50g reaction, scale as necessary.

1) Dissolve 50 g tryptamine in about 1 L of Methanol in a 2 L round bottom flask and stir until material is dissolved. Can use overhead stirrer or stir plate/stir bar. Overheard stirrer is a better option, but stir plate with stir bar works just fine. Might need to sonicate or stir for a while depending on how fine of a powder your tryptamine is.
2) Place funnel on top of 2 L round bottom flask and slowly add 42 g of sodium cyanoborohydride with a spatula while stirring.
3) Place round bottom flask into a concentrated salt/ice water bath with plenty of ice (definitely do not want the ice to melt prematurely).
4) Slowly add 90 mL of acetic acid (glacial). Either manually add slowly, or place addition funnel/separatory funnel above (with ring clamp or some other MacGyver contraption) for addition. Should take about 10 minutes for addition.
5) Now, making sure everything is in solution and solution is cold and stirring really well (don’t want hot spots), add 65 mL of methanol to 65 mL of 37% formaldehyde, mix, then add to stirring solution dropwise. Make sure you go slow slow slow. The addition should take about an hour at the minimum. This should definitely be done with an addition funnel or sep. funnel. They are cheap and worth it.
a. This is the step where impurities will pop up if things aren’t cooled and controlled.
6) During the addition of formaldehyde, keep an eye on the ice bath and when it starts becoming more water and less ice (by a decent margin), change it out and re-make it. It’s handy to just have a 4L bottle of saturated NaCl solution (water+salt until there is undissolved salt sitting on bottom)on hand. Grab some of those large Morton salt things at your local grocery store for $1 each.
7) Once all the formaldehyde has been added, continue stirring on ice bath for 1 more hour, then let reaction warm to room temperature.

Stir at room temperature for 5 hours.
9) Reaction will be complete, now time for the work up.
10)Using a rotovap or some type of MacGyver type evaporation setup (needs to be under vacuum, at 40C or less, rotating is nice), evaporate about 600-800 mL of Methanol. Gotta get a feel for this step, as you don’t want everything to precipitate upon addition of base out or it’ll clog the stop cock of the sep. funnel, potentially.
11)Make up some 50% potassium carbonate solution (in water) and cool it on an ice bath. Slowly add it to solution in a separatory funnel (2 L sep. funnel). Probably about 200-400 mL. Add 200-300 mL of chloroform (you can use dichloromethane but you risk some cyclization). Use pH paper to ensure solution is basic, if still acidic or neutral, add more potassium carbonate solution.
12)Shake, but be careful of gas buildup, be sure to exhaust the sep. funnel by venting. Add in some conc. salt water (50 mL) to help speed up the separation.
13)Keep the bottom layer of organic layer, chloroform(product), then extract the aqueous (top layer) again with another 200-300 mL of chloroform. Add to other chloroform portion and keep on side.
14)Repeat again, for a total of about 1L of chloroform extract.
15)Combine chloroform extracts and wash once with 200 mL concentrated potassium carbonate (cooled on ice bath before addition).
16) Now wash chloroform extract with concentrated salt water solution 3x.
17) Evaporate chloroform down until nothing more evaporates. Go to town on this step, heat up the water bath to about 60 or 70 once you get down to almost no chloroform coming off and let sit on full vacuum for an hour or two.
18)Take off round bottom flask from rotovap and let cool to room temperature.
19)One cool thing at this step is you can stir the light amber oil for about 2-5 minutes, and it will all of a sudden turn into a solid. If left alone it will slowly crystallize on it’s own, but it’s fun to give it a nudge and watch it all crystallize immediately.
20)Purification: There are a few ways to purify material further, either through re-crystallization or column chromatography, or both. If you have access to an HPLC, check your material for purity and decide what you want to do here.
21)That’s it folks. Go get it!


Once you have it down, you can do the whole reaction from raw to product in about 8 hours, with 5 hours of downtime. If you have an HPLC, even quicker, as you can monitor the progress...

 

[Rabidreject]

Okay I’m back guys. I appologise for disappearing. Anyone that’s spoken to me knows I’m going through some SAVAGE withdrawals!!
Okay so I did guess that final yellow oil is good and I did manage to freeze precip some crystals from it once and even dry the re-x’d clear oil that I ended up with on the bottom dried in a vacuum desiccator once AND it is ACTIVE! Haha
I forgot how intense DMT can be! I love it!
Anyway that said - it is going from a pale clear oil to white to yellow and now it’s like a red colour or at least parts of it. It’s v odd.
I will probably re-x it again with something different maybe simple ethanol? or even try just washing it with cold solvent?
Thing is, surely if I re-x’d from heptane, if I re,re-x from heptane will the same shit still be in there?
This is why I’m thinking an alcohol…
Or just a good spray with cold heptane?
I feel like it was SO HARD to turn solid, I don’t want to mess with that!!

I think an A/B and defat is maybe needed.
I tried it once with 7% acetic acid using hexane as a defat but the defat didn’t seem to do much.

im currently following a nifty reductive amination for MiPT using acetone and formaldehyde then reducing with NaBH4 as per the DMT synth and it’s pretty nifty how they do the workup, they salt it straight out of a final acetone extraction after defatting with xylene.
I think maybe I just chose the wrong defatting agent….

I WILL figure it out and I’m learning an immense amount!!
I am getting slightly distracted by buying a 40% mix of nitromethane and DCM so that it can be separated for use as either ones for different uses.
I can’t find 100% nitromethane where I live and in terms of shipping it here, it can’t be above 40% nitromethane but I COULD control the solvent in which it is dissolved and it makes total sense to use DCM!
i know I’ll need more than I have currently ordered but at least I know it’s just DCM and nitro-m. I have tried separating that red nitro fuel and eugh. It STINKS and doesn’t separate well.
You get PLENTY of 9% nitro/methanol but hardly if any nitro but luckily I found at least a slightly better option!
I ended up with some 2,5-dimethoxybenzaldehyde so yeah. Don’t want to waste it!

I do thank you for all your comments - I’ll get there. I know I don’t NEED. a rotary evaporator now but DAM would it be nice!!

Can I ask if anyone has a diaphragm pump for a rotovap? How loud are they in comparison to a single stage rotary vane pump?

 

[Rabidreject]

Oh and I do have film making experience….

I DO want to do it, but at the same time - I want it to be right….the stuff I got as I said has all red bits in it as it’s got older (over days not weeks), I also want it to be accessible - so no rotovap or anything to crystalise at room temp…

 

[Rabidreject]

In terms of this synth, given bits of the product are turning red, would it not make sense to instead of going straight to adding a KOH solution to it, add it to a 5-7% acetic acid solution - protonate the DMT, then defat it with, well whatever works, possibly xylene (hexane didn’t work for me) and then sep that off and THEN go to base and extract with the DCM?
Then do a re-x from heptane? Then into the freezer eventually given I can’t do negative pressure for long as it’s loud!

The oil I end up with AFTER the re-x is really annoying and the majority of the product.

Either the above - OR I guess I could re-x THAT with something else like alcohol? I dunno, it just seems like not a lot is done in the ‘workup’ to get rid of any of the shit that is turning my DMT red over days and taking fucking ages to solidify a goo that doesn’t want to ‘set’ - there has to be an easier way lol

Now I’m not an expert chemist but I do some simple principles lol

I also have a lot of tryptamine to either burn or succeed but no more larger experiments until I can settle it small scale now. It’s pointless…I need to work out exactly how much heptane people are saying when they say LOTS. I’m using probably 20-40x the amount of heptane as there is oil to re-x from.

Also, I’m unclear, do I heat the oil up with the heptane from cold or do I throw the boiling heptane onto the oil and then start heating and stirring in a seperate beaker?

 

[mescalito10]

What defat? There's no fat, as it's not a plant extraction. Or you doing the reaction in a dirty saucepan with some cooking oil left?

You say it's getting red, that's normal if you leave it in open air.

You extract with DCM then evap the DCM as much as possible. Then add to that same flask quite a bit of naphta/heptane, everything done with stirring, both DCM evap and now adding you recrystallization solvent.

Now, there's some goo in your hot naphta that doesn't want to dissolve, you either filter that shit or carefully pour the naphta out, so that you don't pour this goo together with the liquid.

After you have extracted this stuff and put it into a glass, then freeze precipitated all the substance, and there's some yellow or white oil at the bottom, you can use a hack. Pour out the used naphta into a clean bottle. Take your dish, without a naphta now, and let it dry a little bit. Scrape it and move everything into a new beaker, heat that beaker while stirring until you start to smell of dmt, most of the leftover solvent will evaporate in that little time. This hot DMT liquid you can pour into one more glass container, as it cools down, it willl turn into white to slightly yellow wax, you can scrape it after it cools and make a fine powder out of it with a sharp blade.

Pack the powder into an air-tight bag, so it doesn't turn red.

 

[Rabidreject]

Okay yeah that all makes sense.
I mean I have heard of them talking about defatting in the workup from this reaction - I did think it was odd but at the same time Hamilton generally knows what he’s talking about - as do his guests.
It’s strange - maybe he (the self taught chemist that was being interviewed) didn’t mean defat and got the term wrong (it was a self taught chemist but iv looked up the syntheses he’s been speaking of and he was no bullshitter)

Either way, that is a pretty genius hack I would not have thought of! So is this clear oil I am left with at the bottom simply DMT with traces of heptane I can’t get out of it?

Also, I realised - why the heck am I doing this in such a massively oversized RB with loads of space left for air?…not ideal I’m realising.

Also I DID NOT realise it had to be constantly stirred pretty much from the point you extract the yellow ‘goo’ with DCM - that may well have affected things.

And just 1 more thing - I’m really glad you said naptha/heptane as heptane is quite expensive in this country (don’t know if it’s coz I could only find n-heptane or if that makes no difference) but iv loads of fresh, dried naptha. I do understand they are not the same thing - do not mistake me, however, its comforting to know that at a push I can still use that.

Okay so a lot to work on! Thanks for the tips, seriously.

The MiPT synthesis was a failure - well, better put, the workup was a failure but I stupidly attempted it late at night whilst I wasn’t really thinking clearly but at the same time I knew I had a plumber coming today haha
I guess let’s stick to one thing at a time!

Does ANYONE ELSE face these sorts of STUPID scenario’s? It’s probably just me and my bad planning and fucked up life management….
Don’t get me wrong, I would NEVER let ANYONE see any piece of glassware or anything I can’t put with my painting stuff, it’s just the constant getting out, putting away, getting out etc etc - I’m moving soonish to a bigger place so may even have space for a perma-lab!
Anyway just a glimpse into the silliness of my life! This is why I need DMT and other psychedelics because every other time iv taken them off the table with the benzodiazepines and opiates already being off the table, it just doesn’t work for me.

I have been in some of the most savage withdrawals coming off these benzos and the part of that journey where I used psychedelics vs the part where I didn’t is drastically different. It’s more about a sense of it feels like it resets my brain somehow - particularly longer trips, they seem to have a much longer afterglow but there is something about DMT and the worlds it takes me to…

I probably have like 450g of tryptamine left and I’ll be working on a way smaller scale until I can figure it out better…so plenty of time for improvement! lol

I actually wanted to ask you guys something about when you consume n,n-DMT. Someone said to me oh I don’t find smoking it that great and described sitting with his eyes open.
Whenever I smoke DMT the bad trips have been when iv forgotten to close my eyes and I just can’t see or I think I see my hands like turning into roots and it’s deeply unsettling but I find as soon as I shut my eyes, it’s far less confusing and scary - for want of a better word. Just wondered on y’all’s experiences!

 

[Rabidreject]

I just realised I should have said I don’t know what DMT smells like ha

Actually that was something I noticed first about tryptamine - it’s similar plasticky smell.
Does 5-meo-t or 5-meo-DMT smell and taste like shit too? Iv smoked 5-MEO-DMT back when my first ever RC vendor (who was basically just selling shulgins products) from Canada but that was probably like 2005 or something? I can’t really remember it - I don’t remember it being mad visual like DMT that’s for 100% certainty. This was before I knew you could just extract it. lol