SaccharinSlayer157
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Concise, Step by step Reaction Scheme for Dimethyltryptamine
I hope this post is appropriate here regarding my last one was very similar but I feel it deserved its place. Let me know if I'm wrong, I'm new to all
of this.
After scouring the web for hours I think I have compiled the easiest and most OTC method of synthesis. Obviously, everything here is purely
hypothetical and nobody should attempt this synthesis where some of the products aren't legal. With that out of the way...
Tryptophan to Tryptamine:
10g of tryptophan, 250ml of xylene, and 12ml of Methyl Ethyl Ketone were added to a 500ml beaker
Solution was heated to between 60C and 80C until no more CO2 was evolved (Should take between 1.5 and 4 hours)
The solvent was boiled off carefully and the residue was dissolved in DCM
The organic phase was washed with a sodium bicarbonate solution, distilled water, and then dried with anhydrous MgSO4
The DCM was removed and you are now left with reasonably pure tryptamine
Tryptamine to Trimethyltryptammonium iodide:
1.6 g of tryptamine, 40ml of absolute ethanol, 6g of methyl iodide, and
5.5g of anhydrous sodium carbonate was added to a 100ml round bottom flask
The solution was refluxed for 5hrs in a hot water bath
Solids are removed by filtration and washed with absolute ethanol to obtain reasonably pure Trimethyltryptammonium iodide
Trimethyltryptammonium iodide to Dimethyltryptamine:
10g of the trimethyltryptammonium iodide salt and 40ml ethanolamine were added to a 100ml round bottom flask
Solution was refluxed for 20min
Ethanolamine was carefully evaporated off
Resultant Dimethyltryptamine freebase was dissolved in hexane/diethylether
Washed with distilled water and sodium bicarbonate solution
Optionally decolored with activated carbon while hot
Solution was left to evaporate to obtain reasonably pure
Dimethyltryptamine crystals
If anyone has ANY suggestions as to how to make this process more efficient/OTC please feel free to share. I'm posting here specifically for
critiques.
[Edited on 1-10-2020 by SaccharinSlayer157]
[Edited on 2-10-2020 by SaccharinSlayer157]
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karlos³
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Haven't you already posted this under another handle?
Yes indeed you have: http://www.sciencemadness.org/talk/viewthread.php?tid=156197...
Actually for DET and not DMT, but you can take most of our answers for granted to be working likewise.
As for your decarboxylation: MEK is a bad catalyst due to its boiling point.
It will simply escape during the reflux, and your mentioned temperature isn't adequate for this either.
Simply use acetophenone instead.
Your workup needs improvement as well.
Boiling xylene off, alright... and hope that you won't boil off your hopefully formed tryptamine with it, right? 
Just extract into an aqueous layer with acetic acid, then wash that with plenty of DCM to remove the acetophenone, and then precipitate the tryptamine
freebase with ammonia.
Thats how it is usually done.
With your way, you will not be left with "reasonably pure" tryptamine 
Also, DMT doesn't dissolve in an hexane/ether solution, this is done to precipitate the product in a recrystallisation from ether.
If you just want to dissolve it, use only ether(I hope you're not speaking of that OTC starter spray containing both though, because that will
definitely not work!).
Hexane is a very bad solvent, as you need lots of it.
Thats why its so useful to precipitate the product from an ethereal solution.
You definitely need pure ether.
And good luck getting any crystalline product with that workup, even if it would work as intended.
Best you can hope for is an oily substance I would say.
Especially since you include no step to dry your solvents, which is standard practice.
All in all, you have to learn some more, in my humble opinion.
Don't use reasonably pure when it is not reasonable, for example.
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SaccharinSlayer157
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I guess I was a bit overconfident when it came to my yields, especially since I haven't performed any of the experiments myself.  As for using MEK as a catalyst, I just saw a recent post here
https://www.sciencemadness.org/whisper/viewthread.php?tid=31...
saying they got 85% yeilds from MEK and xylene. That's acceptable for me, Unless I shouldn't believe it for some reason. I hear you loud and clear
when you say hexanes are a bad solvent so I'll get rid of that for sure and that tryptamine workup looks way better too. Thanks for the help, I
obviously needed it.
[Edited on 1-10-2020 by SaccharinSlayer157]
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njl
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1. There is a thread on this forum that is specifically about the decarboxylation of tryptophan to tryptamine with various ketones. I believe other
ketones had better yields than MEK.
2. How is methyl iodide OTC? Or ethanolamine for that matter? Eschweiler Clark reaction just uses formaldehyde and formic acid, and you don't have to
deal with over alkylation.
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karlos³
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Also you have to keep in mind, that the decarboxylation is not that simple to get to work as a beginner.
I've seen many people struggle with it, and those who get high yields consistently are usually quite experienced, in general and in special with this
reaction.
Acetophenone works much better in that aspect and it seems to allow even less experienced people some degree of success.
Good luck that you get something out of your first attempt at that reaction.
And, a more OTC ketone catalyst would be carvone, which can be used in its crude form as the ethereal oil of peppermint or caraway, at least it is
higher boiling and success stories exists about it too.
@njl, the standard eschweiler-clarke with formic acid does not work on that substrate, because it is acidic and that results in cyclization due to the
pictet-spengler reaction.
You need NaBH4 and very strict temperature control with good cooling to have success with it.
Ethanolamine is actually OTC in many products, cleaning stuff, baking oven cleaner, whatever, in things like this.
I wouldn't want to use those to purify ethanolamine from though, but it should be possible.
MeI can be made OTC with iodine, methanol and aluminium, all of them pretty OTC as well.
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SaccharinSlayer157
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I had been planning on using chemplayer's method using aluminum foil for the MeI and simply buying the ethanolamine online. I was not aware that
ethanolamine was OTC at all. Does anyone have any specific examples of this? If not I can just look around myself but a headstart would be helpful.
Also, what's the best route to acetophenone? I'm limited when it comes to things like acetyl chloride as most of us are and the only other way to it
that I'm seeing is through the destructive distillation of Calcium benzoate and acetate mixtures.
[Edited on 2-10-2020 by SaccharinSlayer157]
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karlos³
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I've seen it in said baking oven cleaner... but not pure, so forget about this source.
Its contained in similar product, but always impure or in quantities of just a few percent, so better buy this cheap, harmless and nonsuspicious
chemical directly.
The thermal ketonization of calcium benzoate and -acetate is surely one the best ways to make it.
But the purification would surely require you to redistill it more than once to get a clean product with this route.
Although... why don't you buy this stuff too? Because this is the best way to get your hands on some.
And at least you save shipping costs this way, as it is likewise a cheap and nonsuspicious chemical.
You don't need to make acetophenone if you just look out for some essential oil containing a good amount of carvone.
I mentioned peppermint and caraway, those are probably the best choices, although the latter is likely more costly, so just take the former.
Both enantiomers will work just as fine though.
Its not much worse than acetophenone in terms of reactivity for this reaction.
Either buy this or acetophenone, but making acetophenone is unneccessary work if you ask me.
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SaccharinSlayer157
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I appreciate the help and I'll be sure to look into carvone and peppermint oil when I can.
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Corrosive Joeseph
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https://www.bonnymans.co.uk/product-page/monoethanolamine-et...
https://mistralni.co.uk/products/mea-monoethanolamine
/CJ
Being well adjusted to a sick society is no measure of one's mental health
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njl
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I have had success with tryptamine/formaldehyde/formic acid as determined by melting point and activity. The yield was not good. But if this thread is
actually about OTC routes then I don't know what could be easier. I suppose MeI is OTC, but to me OTC means I can go to a brick-and-mortar store or a
consumer website and buy it without any hassle. So by both definitions ethanolamine is OTC, but to me MeI is not.
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karlos³
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Wow, then you are the first person that doesn't got (almost) solely cyclised pictet-spengler ß-carboline as product.
And whatever got produced is not easy to separate from each other, makes me even more impressed that you were able to isolate the DMT cleanly enough
from the beta-carboline to allow for that.
Please some more details, on the conditions, quantity of the used reagents, in special the formic acid, and of course on how you did the workup and
isolation of the desired product from the byproducts?
You should report about that on the hyperlab and vespiary, it will be a sensation!
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draculic acid69
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Quote: Originally posted by njl  | 1. There is a thread on this forum that is specifically about the decarboxylation of tryptophan to tryptamine with various ketones. I believe other
ketones had better yields than MEK.
2. How is methyl iodide OTC? Or ethanolamine for that matter? Eschweiler Clark reaction just uses formaldehyde and formic acid, and you don't have to
deal with over alkylation. |
A local supermarket chain had there own brand of oven cleaner which clearly stated that it contains 10%ethanolamine.
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Texium
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Please take this to The Vespiary. It doesn’t belong here.
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Texium
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Thread Closed
7-10-2020 at 06:46 |
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