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Extraction with Ethanol reflux

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xf-dmt

xf-dmt

Rising Star
Hi there,

I'm wondering if it would be possible to perform an extraction.

I have a reflux condenser, 96% ethanol, powder mhrb ...

is it possible to do a full spectrum extraction if you mix 200mL of ethanol with 20g of mhrb and put it to boil?

1. Is it possible? I think maybe it's not because of the b.p. of the dmt 60º-80ºC ... Could the dmt be decomposed or oxidized at the temperature of 78ºC of the ethanol?
2. If it is possible, how long is sufficient to capture all alkaloids? 3 hours?
3. After doing the extraction for ethanol, can I filtrate and then evaporate it without the reflux, without losing the dmt? I need to acidify?


Look, i've sohxlet extractor, some lab glassware, heating plate, straight condenser, powdered mhrb..
i've pure citric acid, 37% HCl, 5% CH3COOH (acetic acid), ethanol 96%, heptane, naphta, anhydrous acetone, and some other little things...

So, i've try to many times to do sohxlet extraction but without sucess because of clogging..
So I thought about using sohxlet to reflux, and then evaporate the ethanol...
after this i'm thinking to basify and extract with 50ºC heptane..
I'm open to opinions... ty
 
My goal is [post #53]

Trickster said:
So, after many trials and errors here is my best Soxhlet or CSLE tek.

1. Soxhlet alcohol extraction (methanol and ethanol seem to be better than IPA).
2. Distilling and drying the alcohol as much as possible.
3. Dissolution of the extract in diluted phosphoric acid (pH ~4.5).
4. Settling/decanting/filtering the acidic solution.
5. Basifying to pH ~11.5 by adding diluted NaOH drop-wise and checking pH regularly.
6. 6-7 small Heptane/Hexane pulls. Prior to pouring the mixture into a sep funnel I stir it for 10-15 min with a mag stirrer/hotplate on "low" and temp set on 50 C. I prefer Hexane because of its lower b.p.
7. Reduction of NPS until it becomes cloudy. Usually to 1/3rd - 1/5th of the original volume.
8. Slow cooling of hermetically sealed freeze-precipitation beaker. 2 hrs at room temp + 4 hrs in a fridge + 8 hrs in a freezer.

The procedure has been tested several times and it consistently produces ~1% yield. The product looks white and crystalline. No MP test yet, but bioassay results are very positive. 3 different persons were launched into hyperspace using 30 mg each.

Advantages:
- efficiency (most of alcohol and NPS could be recovered),
- consistency,
- high yield,
- eco-friendly,
- good quality product (no need to re-x).

Disadvantages:
- requires some special lab equipment,
- requires certain minimal skills.

P.S. Attached is the product photo. These 850 mg were extracted from 70 g of year-old brazilian mhrb.
Click to expand...


but i can't do sohxlet without clogging like Trickster do.
phosphoric acid can be switched with citric acid, ok?
 
The oft-repeated 60 - 80 C b.p. of DMT refers to a fairly stiff vacuum so there's no need to worry about stability at the temperature of boiling ethanol.

If you look at the soxhlet techniques for cactus, you'll see that ammoniacal ethanol has been used with some success. It may be the case that someone has tried this approach for MHRB but unfortunately my recollection's a bit foggy right now!

There's no reason this shouldn't work - freebase DMT is freely soluble in even 90% ethanol. It also freeze precipitates (at around -25 C) as a concentrated oil from 50% aqueous ethanol...


Do you use cellulose thimbles in your soxhlet apparatus? Why is it clogging? You need some means of keeping the outlet free and even rudimentary sewing skills would allow you to fashion a reusable thimble out of thick cotton or similar cellulose-based fibre. Just make sure you don't pack the soxhlet body higher than the syphon.
 
1º: ty for the light..


downwardsfromzero said:
The oft-repeated 60 - 80 C b.p. of DMT refers to a fairly stiff vacuum so there's no need to worry about stability at the temperature of boiling ethanol.
Click to expand...
I'm confused, the merk index says b.p. 60 - 80ºC ...
source: https://toxnet.nlm.nih.gov/cgi-bin/sis/search2/r?dbs+hsdb:@term+@rn+@rel+61-50-7

What is the DMT b.p. at 1 atm?

downwardsfromzero said:
Do you use cellulose thimbles in your soxhlet apparatus? Why is it clogging? You need some means of keeping the outlet free and even rudimentary sewing skills would allow you to fashion a reusable thimble out of thick cotton or similar cellulose-based fibre. Just make sure you don't pack the soxhlet body higher than the syphon.
Click to expand...

I don't have acess to cellulose thimbles =/ ..
I tried with cotton and also with napkins .. I did it this way: the soxhlet hole was capped with a little cotton ...
so if I get it right, is it necessary to leave an empty space near the hole of the soxhlet? without cotton directly capping the hole?

ill try take some pic's ..
 

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it depends on your soxhlet, some of them are not designed perfectly and don't siphon that well.

You should be able to get it to work without a thimble, just with a cotton plug. I've had success with it. Don't pack it too tightly, make sure both the cotton and the bark are just loosely in there, well settled but not packed. Worst case you might have to just manually force the siphon by removing the condenser and displacing the volume by applying pressure or adding a bit more solvent.
 
endlessness said:
Nowhere in literature does it say DMT's BP at 1 atm unfortunately. I wonder why.... It is definitely above 100c though, people have tested before.
Click to expand...
this information is very useful .. I used to think that the freebase evaporated at 80ºC at atmospheric pressure...

Mindlusion said:
it depends on your soxhlet, some of them are not designed perfectly and don't siphon that well.

You should be able to get it to work without a thimble, just with a cotton plug. I've had success with it. Don't pack it too tightly, make sure both the cotton and the bark are just loosely in there, well settled but not packed. Worst case you might have to just manually force the siphon by removing the condenser and displacing the volume by applying pressure or adding a bit more solvent.
Click to expand...

how you do it ?
i've do now without pack it too tightly and one more fail..
I tried with something that left the hole free but the cotton left the dust to pass ... I tried with enough cotton on the side to see if it did not stick but without success.
 

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I'm almost giving up using soxhlet...

I will try to use it just now as reflux, since the dmt does not evaporate at 78ºC ...
One doubt: if I make the extraction with boiling alcohol, then filter it, and then evaporate it, is it possible to get dmt without oxide in the end?
using a solution of sodium carbonate for dilute for example?
 
It looks like your powder expanded and this contributed to the clogging, along with fine particulates and recrystallising tannins. If you try again, a pre-soak would be in order, perhaps along with sewing the bark into a nice little cotton pouch. Thinking about it, those tannins seem to be the killer. This was an acidic extraction, wasn't it? I still say give the ammoniacal ethanol a go.

Note that most people, even those with soxhlet apparatus, don't soxhlet their MHRB because it's far more amenable to extraction by simpler methods :)

That said, I'm now very much tempted to try running one of my soxhlets with ammoniacal ethanol just to see what happens. The question would be, how much material to use? Small or... bigger? Small goes in the cellulose thimble, larger gets a bespoke cotton jacket.
 
thanks for the support downwardsfromzero.
I decided to use the soxhlet only as a reflux.
> put about 600mL of ethanol 96% + 60g mhrb
> 3h reflux (constant 78ºC)
> cool
> filter 2x with napkin and funnel..
> distilling and drying the alcohol as much as possible (until about 60mL, dont know really)

*photo* (I believe this is a mixture of water, ethanol and alkaloids including nndmt)

> put in an evaporating dish and homemade desiccator
> wait to dry
...
then I'm going to continue with the Trickster extraction like i quote above..
 

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I tried the Trickster's soxhlet tek once with disappointing results.

As for the method, I rolled MHRB in the coffee filters, secured with rubber band and loaded in the Soxhlet.

I followed the tek to the letter and got yield of only 0.1-0.2%
 
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