Im no chemist but I wonder if, should you have the right set-up, you could utilise the difference in the vaporisation temperatures to separate the two?

Yes, absolutely, DMT has a boiling point of 60-80°C, whereas 5-MeO-DMT has a boiling point of 208-210°C. That means that they could be easily separated by sublimation. Even though that's not too hard to do, it's not something everyone neccesarily can perform. I'm therefore looking to find a tek using only solvents and an acid or a base.

that data of dmt boiling point from some literature is wrong though, several tests here in the forum have shown it to be over 100c.. in any case its quite probably under 5-MeO-DMT's boiling point and therefore your general point is correct.

Wiki says 160°C and also 80-135°C, Merck states 60-80°C. What values are correct? Could you link me to the tests you refer to? Thanks!

Ill try to find the links.. But this indication can be seen when everybody was doing the conversion from acetates to freebase by doing a boiling water bath, and there was no loss of freebase. Also IIRC people tried it with freebase crystals..

I am out of dmt but should be doing an extraction soon, I'll attempt to evaporate dmt with boiling water and will post back results. This might take a couple of weeks though

I've researched this a bit, and learned a lot more. The values at wiki and elsewhere is from procedures done in reduced pressures down to 0.03 torr, whereas normal pressure is 760 torr. Using the values I've found in different articles, and employing a nomograph to calculate the values at normal atmospheric pressure, the theoretical boiling point of DMT should be between 360 and 390°C. That's very far from 60-80°C indeed! I don't know how to separate DMT from 5-MeO-DMT though, but I am researching this and many more questions as we speak.

This means that DMT freebase can be in boiling water without any apparent problem. Is this also the case for the salt forms of DMT? I.e. could DMT acetate be in boiling water without any problem?

The easiest way for people at home to do this has to be using prep plate TLC IMHO. This should allow you to separate up to a gram or so of material depending on the plates one uses. Granted this isn't going to be a good method for bulk production...for that I'd use a regular silica gel column and spot checks with TLC.

In any event it almost certainly is going to be cheaper to find an online vendor that will ship you 5-meo.

Peace.

The reason I'm investigating this is because many different types of grass with DMT also contain 5-MeO-DMT. Both preparative TLC plates and silica gel column is a bit advanced (and expensive!) to be done by most home extractors, I would think. I'm therefore looking for other ways to separate the two. But they have so similar properties that I think we will really have to think outside the box.

TLC is as simple as ordering the plates and a black light. Most of people doing extractions already have all the solvents necessary. I agree a full size silica column would be a bit much for the hobbiest, but prep plates could easily be a simple addition to the kitchen chemists' lab.

Peace

The thing is finding a good eluent mixture. DMT and 5-MeO-DMT have awefully similar Rf's in a lot of solvent systems, some exactly the same.

The ones with farthest difference according to literature that I can find are (all silica gel):

t-Butanol-acetic acid-water (70:2:29)
Rf
DMT 0.50
5-MeO-DMT 0.40
(Duttha & Ghosal 1967)

or

t-Butanol-Formic acid-water (21:0.6:9)
Rf
DMT 0.81
5-MeO-DMT 0.71
(Morimoto & Matsumoto 1966)

or

2N acetic acid
Rf
DMT 0.50
5-MeO-DMT 0.60
(Dutta & Ghosal 1967)

Preparatory plates are silica gel on the front of a glass plate.

If the Rf's are close together then one just needs to run the plate longer...of course there is a limit as you could just run your product right of the end of the plate. I must sheepishly admit to having done this in grad school! Started my plate and then began talking to a friend...completely forgot my plate. It was a sad day as this was a nucleoside compound that I had been working on the synthesis of for well over a year at that point. But I digress...

You probably can't separate similar Rf's on a regular TLC strip, but a plate may very well give you enough silica to do the job.

Even if you get spots that bleed together you can use an exacto knife and cut the main region of the two spots out which would yield pretty pure product.

In any event this is not going to be an economical method. Plates are pretty darn expensive.

Here's on source with some 20cm X 20cm plates that I'm sure would do the job...well I'm pretty sure they would. For sure I would be using regular TLC and a very small amount of material to make sure the spots at least start separating before committing a lot of material to this method.

http://www.silicycle.com...c-plates/tla-r10011b-323

There must be a cheaper source out there...this was just a one off google search here as I haven't ordered any plates in years now and was just curious as to a rough price range. IF one could find a source were the cost per plate was $2-$3 bucks this would start becoming an attractive method I think.

Admittedly I haven't done a bit of synthetic work in quite few years now...so if other bench chemists have tried this already perhaps they can point out any potential mishaps in addition to what Endlessness noted?

For what it's worth this method is used to separate close analogs in a Med Chem setting all the time...so I'd be pretty surprised if it wasn't possible.

Yeah Joedirt, definitely the longer you run, the easier distinction it is. The thing is, some Rfs are reported the exact same for some eluents. One would have to check individually the references to see what size was the researchers plate, maybe they just hadnt run it for a long enough distance to see the difference.

Methanol:ammonia at 100:1.5 is not good for separating 5-MeO-DMT and DMT IME. We're using merck silica gel 60 f254 20x20cm .. Spots will fluoresce at 254nm UV light, aiding visualization.

For others running normal plates, they need to find some reagents and other methods for visualization of spots.

Notice we just started a new subforum dedicated to this: https://www.dmt-nexus.me...t.aspx?g=topics&f=75

I will be adding info on TLC, other analysis and more there, over time.

Hey thanks for the link...I don't know how I missed that section?

Anyway I noticed Benzyme has already posted a method for making your own TLC plates. If someone wanted to try this it would surely save on cost.