Thoughts or experiences using Ethyl acetate or n-Butanol on Lazyman TEK

[Psyvoyager]

Hi all, a newbie here.

I have been looking for experiences or tips on using Ethyl acetate or n-Butanol as solvents on Lazyman´s TEK and did not find too much about it. I am just guessing that´s possible because of this paper Internet method for the extraction of N,N-dimethyltryptamine from Mimosa hostilis roots: Does it really extract dimethyltryptamine?, but as far as I understand -with my very limited chemical knowledge- some steps would probably need to be made differently, specially in order to force the precipitation. Any idea about the temperature could be needed with any of both?

I´ve found plenty of references to Ethyl acetate used on cacti, but the few I´ve found about using that or n-butanol on MHRB were only to obtain e-cig liquids, nothing leading to crystals... What steps do you think would be necessary to change on Lazyman´s in order to success obtaining crystals with any of both, Ethyl acetate or n-Butanol?

 

[_Trip_]

You can salt out with EA and or salt out, decant, rebase with a small amount of sodium carb and water evap that, do a mini EA pull then evap again for freebase.

Unsure if EA freeze precipitates. EA can hold a small percentage of water which would really effect freeze precipitation if present.

 

[Transform]

EA would start to get hydrolysed by the lye used in Lazyman's tek. It's often possible to adapt an extraction according to the materials and solvents which one happens to have at hand. The question is, therefore, what exactly do you have access to at the moment?

There has been some discussion on the use of EA in DMT extraction here, mostly in the context of precipitating DMT citrate as "honey oil" by direct addition of citric acid powder to the EA botanical extract.

 

[Psyvoyager]

Thanks a lot for the answers!

@_Trip_, Just to be sure I am getting it right, by salting out with EA you mean after a previous basification or directly without it?

@Transform, Maybe using sodium carb or lime instead of lye would be better to avoid the EA´s hydrolysis?

I am just checking about EA and butanol because they are easier to find in good purity for a good price inside the European Union, not being so easy to find here the kind of Naphtha usually recommended in the forum, which if I got that right should be light Naphtha, aliphatic/C6-C7/Hexane-Heptane-Isomers, and with a boiling point between 60 and 100 ºC.

Plus, after looking a little bit for the risks of each solvent it seems like EA and butanol maybe could be a safer option, specially safer than hexane which seems to be pretty harmful… Anyway been thinking about the possibility of using heptane first, in order to begin with an easy and established TEK, and found some affordable options, both very similar claiming a 95% purity and with the following specs. What do you think, maybe could they fit for that purpose or should I keep on searching for an better source of n-heptane 99%?

Nº1:
Solubility (0,5 g/ L a 20°C)
Flashpoint -1ºC aprox.
Boiling point 87,7-99,9ºC
C-7 Min. 95 %
Color (SAYBOLT) > 30
Density (15°C) 0,690 – 0,698 kg/ L
Distillation range 90 – 100 °
Bromine index < 50
Sulfur < 1 ppm
Benzene < 0.005% vol.
Aromatics Max. 0.005% vol

or

Nº2:
Density (15 ºC) 0,690-0,698 g/cc
Distillation range 90 – 100 °
Color SAYBOLT ≥+30
Not volatile ≤10 mg/100ml
Benzene ≤0,005 %
Aromatic ≤0,005 %
Sulfur ≤1
Doctor NEGATIVE
CORR. Cu (3H. 50ºC) 1
Bromine index ≤25 mg Br/100g

 

[doubledog]

Butanol could be an interesting option for a solvent, but I would expect some issues in extraction due to its partial miscibility with water.

 

[Transform]

Those two heptanes look practically identical so you might as well choose the cheapest one. Naphtha equivalents are very easy to find in some parts of Europe, as wasbenzine/waschbenzin, or wundbenzin if you want pharmaceutical grade.

Besides n-butanol, n-butyl acetate seems fairly promising although I can't point to any specific successes with it. It does smell better than butanol, for one thing - if you don't mind the smell of bananas.

 

[_Trip_]

Salt out would mean after you base and pull with EA you would then add a compatible acid that would force the dmt to selectively precipitate out of the EA i.e citric acid. A dry tek would be more ideal if using EA.

So basically do the hielo tek then base the "dmt honey goo" in a small amount of sodium carbonate/water then evap, pull with EA, decant and evap the EA.

 

[_Trip_]

Keep in mind I'm not sure how well it would crystalise when evaping the EA. It could form polymers but this wouldn't be an issue. If it does it would still likely solidify to a wax or you might get beautiful crystals.

 

[Transform]

Maybe using sodium carb or lime instead of lye would be better to avoid the EA´s hydrolysis?

A dry tek would be more ideal if using EA.

A lime "dough" has been used for this before, which is what @_Trip_ is referring to by "dry tek". Lime + EA followed by citric acid for DMT citrate "honey" recovery counts as a more or less established route. n-Butanol would still be experimental by comparison.

Keep in mind I'm not sure how well it would crystalise when evaping the EA. It could form polymers but this wouldn't be an issue. If it does it would still likely solidify to a wax or you might get beautiful crystals.

We've yet to see reports of DMT freebase recovery by evaporation of EA so it would be interesting to find out how it goes, albeit a bit of a shame to lose the EA to the atmosphere.

 

[_Trip_]

albeit a bit of a shame to lose the EA to the atmosphere.

Agreed ideally it would be better if you could get naphtha, Psyvoyager.

 

[Transform]

Agreed ideally it would be better if you could get naphtha, Psyvoyager.

Or a rotary evaporator, if you're a dedicated fan of labware

 

[Psyvoyager]

Thanks for the info! I think I will definitely leave the more complex experiments with EA and other solvents for later to begin with hydrocarbons first.

@Transform I´ve seen about waschbenzin and wundbenzin, but waschbenzin looks like it can contain literally anything; wundbenzin seems more secure but I could not find any proper fact sheet with the composition, some sellers claim they send a batch-related analysis with each purchase but seems like there is no way to know it before buying.

Found this page with some name equivalences for naphtha in different languages, very useful as an orientation even not being totally accurate:

Learn Fire training and safety - International Fuel Names

And after digging on googling synonyms for a while finally found some sources of Naphtha on laboratory reagent grade available in my country Mostly calling it Petroleum Ether and 40/60, but also found some slightly expensiver 60/80.

So, the main difference for that matter between a 40/60 and a 60/80 Naphtha/Wundbenzin/Petroleum ether would be the higher flammability of the first making it more dangerous plus the quicker evaporation of it causing a bigger solvent loss in each pull, right? Or would be anything else important to consider?

And the main difference between using those and heptane would be heptane being a slightly less effective solvent for the vegetal material, so requiring more pulls leading to smaller yields on each one to reach the same amounts of spice, or is there anything else?

 

[Transform]

Thanks for the info! I think I will definitely leave the more complex experiments with EA and other solvents for later to begin with hydrocarbons first.

@Transform I´ve seen about waschbenzin and wundbenzin, but waschbenzin looks like it can contain literally anything; wundbenzin seems more secure but I could not find any proper fact sheet with the composition, some sellers claim they send a batch-related analysis with each purchase but seems like there is no way to know it before buying.

Found this page with some name equivalences for naphtha in different languages, very useful as an orientation even not being totally accurate:

Learn Fire training and safety - International Fuel Names

And after digging on googling synonyms for a while finally found some sources of Naphtha on laboratory reagent grade available in my country Mostly calling it Petroleum Ether and 40/60, but also found some slightly expensiver 60/80.

So, the main difference for that matter between a 40/60 and a 60/80 Naphtha/Wundbenzin/Petroleum ether would be the higher flammability of the first making it more dangerous plus the quicker evaporation of it causing a bigger solvent loss in each pull, right? Or would be anything else important to consider?

And the main difference between using those and heptane would be heptane being a slightly less effective solvent for the vegetal material, so requiring more pulls leading to smaller yields on each one to reach the same amounts of spice, or is there anything else?

Well, as @floreal____ recently observed, heptane would likely give a cleaner-looking product, so more pulls needn't be a bad thing.

Wundbenzin should correspond to some established range within a pharmaceutical standard, so a bit more digging around will likely reveal what that is. Waschbenzin should at least adhere to a standard for maximum permitted content of n-hexane, benzene, and other aromatics, but the standard for low-volatility residues may be less stringent. The stuff in plastic bottles, as well, would be better carefully distilled before use.

Your observations about the 40/60 pet. ether naphtha are indeed correct - the rate of evaporation can get quite inconvenient, so it would best be reserved for room temperature pulls if anything. It might be good for defatting during an A/B of, say, acacia material as well (MHRB doesn't really require defats). I wonder if this inconvenience is what makes it cheaper than the 60/80 stuff? I'd go for the 60/80, since it would also be more useful for recrystallisations.

Uh-oh! Crummy solvent alert:

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Good work on the international synonyms, btw - that's totally one of my favourite fields of learning!

 

[Psyvoyager]

Wundbenzin´s standard seems to be fixed by the DAB, Deutsches Arzneibuch or German Pharmacopoeia, but the whole document seems to be not available anywhere in open access… I just found that at least benzene is totally banned from the current official wundbenzin DAB formulation, and also this work https://www.dguv.de/ifa/forschung/projektverzeichnis/ifa2098.jsp which claims it´s a mixture of saturated C6 and C7 hydrocarbons obtained from petroleum in a boiling range of 30°C to 85°C -something kind of strange as the most common wundbenzin found on the web is 40/65, a boiling range which in theory should be composed mostly by C5 and C6, plus only much smaller portions of C7, or am I wrong?

 

[Transform]

Wundbenzin´s standard seems to be fixed by the DAB, Deutsches Arzneibuch or German Pharmacopoeia, but the whole document seems to be not available anywhere in open access… I just found that at least benzene is totally banned from the current official wundbenzin DAB formulation, and also this work https://www.dguv.de/ifa/forschung/projektverzeichnis/ifa2098.jsp which claims it´s a mixture of saturated C6 and C7 hydrocarbons obtained from petroleum in a boiling range of 30°C to 85°C -something kind of strange as the most common wundbenzin found on the web is 40/65, a boiling range which in theory should be composed mostly by C5 and C6, plus only much smaller portions of C7, or am I wrong?

Branched chain isomers will have lower boiling points,

Heptane has nine isomers, or eleven if enantiomers are counted

plus there must not be more than 5% n-hexane in the mix, quite possibly far less by this (inaccessible?) standard. [I wonder if you could try asking at a public library?] But 65°C still seems far lower than the boiling point of the major isomers of heptane, indeed. Perhaps Wundbenzin is largely 2-methylpentane or similar?

And yes, the benzene/benzine similarity is rather annoying, tempered only by the German name for benzene being, instead, benzol.

 

[Ruffles]

I have tried n-butanol in an acid base extraction of Mimosa powder. Not good at all compared to other nonpolars. It pulls a lot of water from the polar fraction and it is very difficult to FASA because of it. Forget about drying it without a fume hood, smell is disgusting.

 

[Psyvoyager]

[I wonder if you could try asking at a public library?]

This was one of my first thoughts being a librarian myself hehe but unsuccessful in my country´s regular public system. It might be easier to find it within the German system, I guess. Perhaps someone there could try. And maybe I might still have a chance to access it through a college system from here, which often has broader and more specialized databases.

 

[Transform]

I have tried n-butanol in an acid base extraction of Mimosa powder. Not good at all compared to other nonpolars. It pulls a lot of water from the polar fraction and it is very difficult to FASA because of it. Forget about drying it without a fume hood, smell is disgusting.

I'd say n-butanol maybe deserves a 'last chance' in a drytek, but the odour really is quite a disadvantage. It might work with a dry SC tek - but why bother when acetone, ethanol or IPA are likely to be far more readily available?