So I bought a vacuum chamber…

[Osmosis Vanderwaal]

Heptane boils at like 92°C and chloroform boils at 61°C, so a 50/50 mix would boil at 77°C, 15° less than heptane alone. -1 barr is defacto perfect vacuum. A rotary vane pump can only achieve -0.95 barr or so, that last30 torr or so is where the real action happens. I don't think running the pump disconnected for a couple of seconds is going to release many hydrocarbons . The oil itself is likely a hydrocarbon most are.

 

[Rabidreject]

Ah okay. I get you - this lines up with the advice to put the chamber on or near a mild heat source (I just placed it on top of my heating mantle and put the thermocouple between them and set it to 50c - then pulled as much of a vacuum as I could.
To be honest, I’m not sure this gauge actually goes up high enough to register the vacuum at its highest coz it tops out pretty quickly but I found if I left the pump on for a while longer after it had topped out, I was getting considerably more bubbling at the latter stages.
Im getting there, for sure….

 

[Rabidreject]

Surely all negative pressure is measured in - numbers? This is what ALWAYS confuses me.
Here is the pressure gauge on top of my vacuum chamber - that I filled with a layer of anhydrous MgSO4 and just pulled a vacuum and left it all day (topping up - or down ) the vacuum when the gauge started going back towards 0. Very slowly admittedly.


But to be fair, I woke up this morning to look at the tub that I thought was going to work (the picture I posted above about 5x by accident!)
I found a waxy, mainly white but ever so slightly yellow, scrapable substance! Whoop whoop - this is a synth I have been TRYING my hardest with for nearly 6 months now.
GRANTED - 6 months ago, I knew FUCK ALL about chemistry, aside from what I learned in GCSE chemistry (where the teacher pulled a vacuum ONCE - and now 30 years later, f knows why!) and also some of the principles that I learnt extracting DMT. This is the whole reason I got interested in organic chemistry but OMG what an ABSOLUTE BRAIN SCRATCHER this has been!!!!

Boom -

Okay - now I need to re-x the rest of the oil from the previous step

Thank you SO MUCH for all your really helpful responses!!! The whole way along, the odd person, here and there have given me tips - particularly regarding doing it under non acidic conditions using standard borohydride and not STAB.

Next to do a video, I guess….

 

[Rabidreject]

I really cannot tell you how happy I am I got this done, from having NO scientific knowledge - other than basic high school chem (of which I paid NO ATTENTION and was in the ‘dumb kids group - couldn’t possibly be we were just not interested!) AND more relevantly information from having done bark extractions a lot BUT I found that I HAD to think of it as completely different and even at parts where I thought at first I could compare, I really couldn’t - THE closest thing to the extraction is the second last step where the synthesis told me to simply evaporate away all the hexane but I altered it to do a freeze precipitation as I had the knowledge it was a hydrocarbon, I knew that naptha is a bunch of different non specific hydrocarbons and I put 2+2 together.
It really was easier for me to just know it’s a TOTALLY seperate process…

If I were to go back in time - or if you are reading this thinking oh it’ll be cheaper to setup a whole lab and synthesise DMT from scratch to sell - or even to ingest, I can assure you it’s not. Iv said the whole way through this isn’t why I am doing this…it’s a personal quest for knowledge.

I would also imagine that most folks who would be attempting to do this would be doing so in spare time, maybe at a lab you are working at or are an undergrad chem student or even post grad and are doing a little extra ‘work’ on the side - THAT may well be cheaper, but starting from scratch? Nah…don’t bother, not for a first synthesis anyway.

If I had ACTUALLY bothered to compare the structures of DMT with something like mescaline - I probably would have seen that mescaline is a simpler molecule, some of the psychedelic amphetamines as well would be an interesting one - which is why I’m hesitant to use the small amount of nitroEthane I have, making standard r-amphet.

Aaaanyway - I do intend to try this on a larger scale but I want to see if I can get some more out of the original oil from the step before this…

This isn’t as elegant chemistry as the indole route, I would say BUT much easier and I would be interested to see if doing it with STAB obviously under acidic conditions would make it easier to crystalise at the end coz that bit has been an ABSOLUTE ball ache!

Mind you, not having a suitable lab grade desiccator probably did slow me down some as well as not knowing the difference between a vacuum desiccator and a vacuum chamber! So I did bodge the last bit a little by not pulling AS strong of a vacuum as I’d have liked BUT sitting it on top of my mantle at 50c….it did work and as you can see this morning I was FINALLY left with the waxy scrapable substance at the bottom and the crystals that formed from the freezer around the edge.
Next time I would also try to use a crystalising dish instead of a beaker and I would also make sure I do it from a warm oil bath as well, just really slow down that cooling process as much as possible.
Oh and more bloomin heptane!! I used n-heptane as it was all I could find but learning more about heptane today I can now see why some other syntheses iv seen of this nature use like 1,2-hexane which is actually a type of heptane.

Gah - it really is, the more I learn, the less I seem to know!!!

 

[Osmosis Vanderwaal]

No no. Hept, 5. Hex=6 heptane has 5 carbons and if it's cyclic it looks like home plate. Hexane has 6 carbons and cyclohexane is shaped like a stop sign. I've never seen a cycloalkane pick up a carbon and add a side. I think it can be done with a ring opening but I don't think you will see it spontaneously do that

 

[Rabidreject]

Oh okay, to be honest it was just what I read on Wikipedia as I was wondering what n-heptane was and if this was why I was having issues. Take a look at some of the other isomer names…this is why I was confused as you say

 

[Osmosis Vanderwaal]

So your gauge. At the bottom it tells you what unit you are measuring. The inside marks are Barr. 1 Barr= 14.7psi, 760 torr, 29 INCHES Of HG (mercury). All of these numbers are 1. 1 atmosphere. The air pressure at sea level. If you could max that gauge completely out you would be pulling a perfect vacuum. Like I said, a single stage rotary vane Should pull -0.8-0.9 Barr, 28" of mercury or a little over 700 torr

 

[Rabidreject]

That all makes sense yeah….


I really cannot tell you how happy I am I got this done, from having NO scientific knowledge - other than basic second school chem (of which I paid NO ATTENTION and was in the ‘dumb kids group - couldn’t possibly be we were just not interested!) AND more relevantly information from having done bark extractions a lot BUT I found that I HAD to think of it as completely different and even at parts where I thought at first I could compare, I really couldn’t - THE closest thing to the extraction is the second last step where the synthesis told me to simply evaporate away all the hexane but I altered it to do a freeze precipitation as I had the knowledge it was a hydrocarbon, I knew that naptha is a bunch of different non specific hydrocarbons and I put 2+2 together.
It really was easier for me to just know it’s a TOTALLY seperate process…

If I were to go back in time - or if you are reading this thinking “oh it’ll be cheaper to setup a whole lab and synthesise DMT from scratch to sell” - or even to ingest, I can assure you it’s not. Iv said the whole way through this isn’t why I am doing this…it’s a personal quest for knowledge….

Now - how do we attach two ethyl groups to tryptamine instead of the methyl groups? Would performing it in ethanol instead of methanol and with acetaldehyde instead of formaldehyde work?

 

[Osmosis Vanderwaal]

Jus) Diethylamine and ethyl ether probably

 

[Rabidreject]

Gah, diethylamine is hard to get! For a very specific reason…if there is an easy way to make it please do make me aware but from what iv seen because of LSD it’s pretty hard to get…

 

[Rabidreject]

Does anybody know if what is said on that n,n-DMT synthesis on hamiltons show about STAB being a better reducer of carbonyls, than say, NaBH4?

Would that result in the workup being less…sloppy…it just seems particularly soggy or ‘oily’ with the synth I’m using.

I did get success but with a view of ‘improving’ the wetness of it once I’d transferred it to a smaller silicon container, I put the vacuum desiccator on top of my mantle but put the heat slightly too high and it melted! Haha just my luck…now I can’t seem to resolidify. Maybe it takes a while…I dunno.
I crushed up the MgSO4 that I made yesterday and for the first time experienced it blown everywhere with decompression! Whoops. Lesson learned.

anyway, I have 3x more of them that have gone from boiling to cooling in an oil bath this time. It just takes - SO MUCH n-heptane to even get anything out of the yellow oil of evilness from the step before! Maybe I wasn’t heating or mixing it aggressively enough….

We’ll see, it’s all a 20g of tryptamine experiment so I know what I need when I do the other 450g!

 

[Rabidreject]

Maybe 20g, or 21 to be fair, in 500ml of methanol just wasn’t enough or maybe it was too much…
Thing is, that I actually got more of the yellow coloured oil from the first attempt whereby it went a lot warmer than the second.
I had to mix the oils from the stage before together due to having dropped a jar of branston pickle onto one of my erhlenmeyer flasks with it in! Typical lab problems ay?! Haha

 

[Rabidreject]

If it doesn’t work this time, I’m giving up, and buying the 3,4,5-trimethoxybenzaldehyde I need to perform the Henry reaction on it using nitromethane or nitroethane. I made sure it is the last thing I obtain this time….
As opposed to this; where I’m stuck with loads of tryptamine!

 

[Osmosis Vanderwaal]

The fact that it doesn't want to dry means it isn't particularly pure. What color is it? How did you clean it? What was your solvent? I haven't read this thread thoroughly, and I'm not into DMT and haven't read any synths, but for me, the strongest reduction agent happens to be free and I already have it and you probably do too. It's lithium

 

[Rabidreject]

Oh no it’s fine now….i was just being impatient….also I hadn’t made my own anhydrous MgSO4 at that point. Once I basically just did what the synth said it worked fine!

 

[Rabidreject]

Yeh but I would want LiAlH4 to be fair and don’t much fancy making it….

I havnt beeen doing chemistry for more than 6 months so one step at a time ay?

Some people say that STAB is good for reducing carbonyls so I’d be interested in trying that another time.

The oil was just off clear and it dried to a waxy, just off white scrapable substance that smells exactly like all the extracted DMT iv had in the past.

Next I would be interested in making mescaline, iv been slowly saving up the reagents for a while now. Just need the aldehyde now

 

[Rabidreject]

Oh and the LiAlH4 I need which is annoyingly hard for me to get.
I am considering using an amalgam - not that I know much about it yet. I just saw someone using it to reduce md-p2p and have definitely heard people use it for the Henry reaction or sorry, I should say for the reductive amination of md-p2p. Oh and I’m talking about applying that to the reduction of the precursor for mescaline - which is made using the Henry reaction (it temporarily escapes my memory as I’m half watching a doc on Madoff hehe)

It VERY much depends on what my usual site I get my cheap borohydride from - if they have the mercuric (chloride?) don’t quote me on that - I know it’s mercuric something or other.
Honestly, it’d be a lot easier if I could just find someone to sell me 50g or so of LAH.
I don’t need much to be fair as I don’t reeeaaaally tend to sell, I’m simply interested in cutting out the middle man as much as possible.

I started with n,n-DMT from tryptamine as it’s simple and also the bark of a tree cannot be particularly sustainable.
I see DMT pens and shit in the cannabis community these days and I HIIIGHLY doubt even 1% of that is synthesised and I’m not too sure why….
It’s worth more than coke…the precursor is easy to get and pretty unwatched - at least in this country and once you have a lab (def the most expensive part in this equation - which may be part of my answer but honestly, I think it’s just easier to pull down trees…) oh well. I guess it’s a pretty niche market still but it is getting more and more heard of. When I first extracted it - only psychonauts even knew what it was. Now I see the pens in particular, for sale all the time.

Anyway - thanks for all the help with this guys…it really is MUCH appreciated.