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DMT distillation log

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I have an idea...try changing the setup.

select a high boiling solvent, and use a reflux app, with something like a friedrich to condense (and optionally, an aux. condenser connected to the friedrich outlet). I used this setup for the decarboxylation of tryptophan with nothing more than mineral oil, tryptamine had sublimated on the friedrich, and it was identified with IT-MS.

the friedrich acts like a coldfinger.
 
benzyme said:
I have an idea...try changing the setup.

select a high boiling solvent, and use a reflux app, with something like a friedrich to condense (and optionally, an aux. condenser connected to the friedrich outlet). I used this setup for the decarboxylation of tryptophan with nothing more than mineral oil, tryptamine had sublimated on the friedrich, and it was identified with IT-MS.

the friedrich acts like a coldfinger.
Click to expand...

That may work, if the friedrich should provide enough surface area to allow the tryptamine to solidify a bit further. I had the worst luck testing it for sublimation in the sense it would turn from a vapor and into a hot oil and run down the sides.

Giving more surface area for cooling and perhaps more immediate cooling will change the outcome dramatically. I have a CO2 tank on hand and a dry ice maker on the way (finally). Perhaps if I give it an everything or nothing shot I'll have some better data to work with.
 
I have a large assortment of vigreux columns, I have a few in particular that have hollow glass 'cones' that simple into the column to allow air cooling. a 200mm column may work prior to the friedrich condenser to dispatch excess solvent vapors.

Thanks for the advice benzyme! I never thought about refluxing it onto a condenser!
 
I think Spiritofspice was talking some sense with the glycerol idea. The boiling point of 290C is not a problem if you're aiming to vaporize DMT from it. The glycerol doesn't even need to be boiling. That might combine well with Benzyme's suggestion of condensing in a Friederich's. Then it's just a matter of ensuring the coolant in the condenser is flowing at an appropriate rate to do its job.

Note that heating glycerol with oxalic acid produces formic acid; oxalates are present in many plants - fill in the gaps from here.
 
Spiritofspice said:
How about fractional distillation?

The glycerol boils at 290c I think the BP of DMT is 160c the dmt should carry over between 160c to 185c
You could discard whatever is collected before 160c then maintain that temp to vaporise the DMT and collect in theory the dmt freebase.

I would run the rxn as follows.
Add bark and water and caustic heat and reflux for say 1 hour.
Add glycerol 2 times the total volume of the solution.
Reflux again for another hour at 150c.
Set up for fractional distillation discard everything that comes over before 160c
Collect everything that comes over after 160 and keep going to say 185c
[...]
I'm just not sure how glycerol would react with the caustic.
I think it's made by using alkaline solutions so it shouldn't degrade any more.
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I'll mention this to my neighbour's cousin's friend - with the reflux setup it might prove interesting. Best make a tea and filter out the bark though. That would prevent some of the inevitable scorching that would result from using Spiritofspice's method.

You would have to run your condenser just cool enough to get the dmt vapour to form an oil to be able to collect it.
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There's not necessarily anything wrong with collecting solids in a condenser...
(N.B. - bark contains oxalates, hence the previous mention about glycerol+oxalic. Glycerol+caustic will be fine. Although it will probably etch your glassware a bit.)
 
I can't help but to feel like that would be a nightmare.

How I would carry out the proceedure in short will probably go a bit like this:

Extract DMT from basic solution with methylene trichloride, rotovap off the solvent. Remove alkaloids with heptane and add to a flast of pre-heated dimethyl-sulfoxide. Distill off heptane, and any other fractions not needed. Remove distillation head and setup a friedrich condenser cooled by CO2 chilled DMK fed by a parastaltic pump. The condenser will rest on a 200mm spiked vigreux column. I may add cyclohexanol (as opposed to say tetrahydrofuran or dimethylformamide) to help push DMT vapors up the column if all else fails.
 
benzyme said:
i'd be worried that acetone would chew up the tygon.
ice cold water pumped through the friedrich should suffice
Click to expand...

Yeah it probably would. I was hoping near frozen acetone wouldn't be as interactive, maybe ethanol ;)
 
Looking back at this now knowing how vaping works, the idea with glycerol seems likely to create a terrible caustic fog, which would fit with 1ce's descritption of "nightmare".
 
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