DMT and other tryptamine synth questions….please help…

Rabidreject

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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

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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?
RabidrejectWhat 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

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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.
mescalito10Okay 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

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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.
mescalito10I 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
 

Rabidreject

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Oh one more thing sorry guys…

if I try to salt out the freebase DMT I have using acetone and fumaric acid, will it pull the impurity with it? Surely not right?

I do really want to try the probably slower onset of a subcutaneous injection or even the difference between that and an IM injection but I OBVIOUSLY need it to be white and purified lots before doing so…
 

mescalito10

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Oh one more thing sorry guys…

if I try to salt out the freebase DMT I have using acetone and fumaric acid, will it pull the impurity with it? Surely not right?

I do really want to try the probably slower onset of a subcutaneous injection or even the difference between that and an IM injection but I OBVIOUSLY need it to be white and purified lots before doing so…
RabidrejectMy man don't do that, just take harmalas or some other maoi and eat if you want a slower onset, more mellow trip. Or eat harmalas and then take small tokes of dmt dissolved in vaping liquid straight out of a vape.
 

Rabidreject

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Why not? Personal bias against injection?
I’m not wanting to commit to a pharmhuasca trip because it is Looong but I’m historically used to injecting far less pure drugs - oh and way more dangerous and addictive.
It’s an ROA that looks REALLY interesting….have you not read the shulgin reports? Or others, as long as I can get it pure enough…that would be my main concern but again having said that iv shot up (into muscle) some HORRIBLE street heroin in my time!
Im not saying anyone else do it, or condoning it but it is my preferred ROA.
Plus there is no addition of an additional molecule - which ultimately WOULD change the feel.
I actually did buy a Syrian rye extract on eBay and have taken that before smoking but honestly? Didn’t do jack…and it’s a notoriously annoying one to extract as far as I’m aware. Lots of fat apparently (this time it is fat!)
I would say an oral ROA is my least favourite.
This is why I want to find a way of synthesising DET from tryptamine via reductive amination….it looks like a fantastic drug!
I will retry the MiPT one at one point….

I also won’t try salting it straight out most likely but I will be salting some of the red shit hoping too rid it of the colour
 

Rabidreject

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Is my thinking not valid that plant extracted DMT has never turned this colour when put in the exact same tub. Okay not the best storage option unless it’s totally packed but still, surely if this one is going red and the extracted stuff never has there must be some sort of impurity in there?
Or does synthesised DMT just react differently BECAUSE it is more pure and therefore maybe less protected and bound up in things like fats like the extracted stuff might be?
just seems strange that’s all…
 

Rabidreject

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So I’m having another go at it….

I started it yesterday evening with 10g of tryptamine. I ended up leaving it in my water bath but not turned on and then plugged it and put a tea towel over it (intending to quench it this morning).

So I went to bed, started drifting off and ‘WEEE WEEE WEEE WEEE!!!!!’ - fucking fire alarm kept going off!!

I am assuming that I should have quenched it straight away because when I went to quench this morning nothing happened?
Not exactly sure about why….so if someone could enlighten me that would be useful.
Last time the fire alarm did go off when it was quenching at 35c - seeing as it’s a heat and a CO Detector, I’m not entirely sure why hydrogen generation (although dangerous if enclosed - which it never is), why would this have set off my fire alarm OR is it just coincidence and my fire alarm needs changing?
Last time it went off, it was quenching in the water bath, whilst I was in a different room vaping DMT - so honestly, not sure if it was the plasticky type vapour from the DMT from the smoke detector in the lounge OR if the hydrogen generation triggered the kitchen one. Very odd and has scared the living shit out of me a couple of times now!!

Secondly - I just did the whole basifying, adding DCM and extracting and I found after basifying and adding to a sep funnel, I added a little DCM and after turning upside down and venting, the DCM (now a yellow colour) droplets all sank to the bottom showing two layers. At the same time, in the other layer, there were some white bits that looked like small crystals or an emulsion.
So I kept adding DCM and eventually it got to the point where it seemed to flip upside down - iv never seen this before, the DCM (which now wasn’t yellow at all and looked like it contained the emulsion) stayed on the top layer.
I have never seen this happen before and it confused me - I drained off the original RM that was left into a ‘junk container’ and then drained the weird sort of fatty looking DCM into an empty bottle to distill and reuse.

I have NO idea what the white shit was floating in the mix when I first added the base - I wasn’t sure if it was KOH that had partially crashed out and so didn’t want any in the final DCM that is currently reducing under stirring and a tiny tiny bit of heat.

Also, why did the DCM start by sinking to the bottom of the sep funnel and then at the end it was on top?
Could it be that picking up the DMT along with whatever junk we are getting rid of in the heptane re-x, gives it ‘weight’ and so it sinks.
Maybe after I had added 3x25ml portions, there was no DMT to pull out of the RM and so it just sat on top?

This is really the first time I am paying close attention and writing notes for everything to be honest….

I think my yield so far is like 1% hahaha

I’ll get there!

I still find it fucking odd that the DCM started by being the bottom layer and then just stopped sinking and sat on top!!

Either way, it very much looks like the DCM has finished evaporating (using a fan and stirring), so I’m gonna go re-x
 

Rabidreject

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Okay so I have been doing some reading my friends….
Someone said, what fats would be in there, why do a defat step after acidification?
This is what I found…


In a reductive amination reaction involving tryptamine, formaldehyde, and sodium borohydride, a defat step is often performed to remove non-polar impurities that may interfere with the reaction or contaminate the final product. Here’s a detailed description of why this step is necessary and what types of "fats" (non-polar compounds) might be present:

### Why Perform a Defat Step:

1. **Removal of Non-Polar Impurities:**
- During the synthesis, non-polar impurities such as unreacted tryptamine, any organic byproducts, or residues from previous steps can be present. These impurities can affect the purity and yield of the final product.

2. **Enhancement of Product Purity:**
- Removing these non-polar substances ensures that the desired product is obtained in a purer form. This is particularly important for analytical characterization and subsequent applications where high purity is crucial.

3. **Improvement in Reaction Efficiency:**
- By removing substances that might interfere with the reaction, you can improve the efficiency and selectivity of the reductive amination process. Non-polar impurities can sometimes act as inhibitors or react with intermediates, leading to side reactions.

### What "Fats" Might Be Present:

1. **Unreacted Tryptamine:**
- Tryptamine itself is relatively non-polar and may not completely react with formaldehyde. Any remaining tryptamine would be considered a non-polar impurity.

2. **Organic Byproducts:**
- During the reductive amination, side reactions can produce various organic byproducts. These byproducts can be non-polar in nature and need to be removed to purify the target amine.

3. **Residual Solvents:**
- If organic solvents (such as those used for dissolving tryptamine or facilitating the reaction) are not fully removed, they can contribute to the non-polar content in the mixture.

4. **Intermediate Compounds:**
- Intermediate species formed during the reaction that do not go on to form the desired final product can also be non-polar. For instance, intermediates formed from partial reduction or condensation steps can be non-polar and need to be extracted.

### Typical Defat Procedure:

- The defat step usually involves washing the reaction mixture with a non-polar solvent such as hexane, petroleum ether, or a similar solvent.
- The non-polar solvent selectively dissolves and extracts the non-polar impurities from the reaction mixture, leaving behind the more polar product in the aqueous or polar organic phase.
- After separation, the non-polar layer (containing the impurities) is discarded, and the polar layer (containing the product) is retained for further processing and purification.

In summary, performing a defat step in the reductive amination of tryptamine with formaldehyde and sodium borohydride is crucial for removing non-polar impurities, thereby enhancing the purity and yield of the desired product. The non-polar "fats" in this context primarily include unreacted starting materials, organic byproducts, residual solvents, and intermediate compounds formed during the reaction.

Okay so I won’t lie…I asked chatGPT and when it first spat out an answer I thought it was talking bollocks coz it was talking about the fats fucking with the reductive amination, however, when I read on - it did have some points…which were valid.
It is something I would like to try, it would be useful to not be the only guy in the world with red DMT! Haha, Thing is it still SPANKS any extracted DMT iv ever extracted. Seems much more potent but still - why is it going red when this is not something that is commonly reported.
I do have more on the go so it may well just have beeen that first rxn but still chatGPT made some points…

I also heard it in an interview Hamilton did tbf! Ha
 
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