• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

So what is the best solvent for recrystalization of DMT?

Kalitechnik

Kalitechnik

Established member
Hello fellow chemists. As i am learning more and more i came across very nice educational piece on recrystalization.

The science says that the best solvent for recrystalization is that in which our product (and i am want to know about dmt) is insoluble in room temperature and below, and becomes soluble in higher temperatures?

And that got me to think which solvent it will be? I have not knowledge at all about it, but i believe we should have some experienced chemists here who might know the answer. I am all ears.
 
I just did some searching and found this outstanding reaserch. Do not understand it yet at all, but looks like @Samvidbuho chose heptane for his crystalization, and with such a vast knowledge there might be a reason to it. Is HEPTANE the best solvent of choice for recrystalization?

Here is the amazing post

Solubility Studies 2: The Thermodynamics of DMT Crystallization - Freebase Solubility Curve

For my 2nd solubility study, I examined the solubility of DMT freebase in n-Heptane over a range of temperatures (20C - 105C). Only the preliminary results are in, but I wanted to share anyway because I find the data too exciting. I've wanted to know this for years ! The Word document...
forum.dmt-nexus.me forum.dmt-nexus.me
 
Looks like the answer was right in front of my eyes.

Recrystallization - DMT-Nexus Wiki

wiki.dmt-nexus.me wiki.dmt-nexus.me

"A good recrystallization solvent for DMT is heptane. DMT is not very soluble in it at room temperature but quite soluble as we add heat. Most common spice impurities, however, are not very soluble in it at all and can thus be separated via simple decanting."

Feeling a bit ashamed ;)
 
its not that heptane is good, or the best. but heptane is extremely similar to hexane, and hexane is a known effective solvent for crystalizing or extracting, its also a major component of shellite. In all chemistry its generally recommended to transition from hexane to heptane where possible, using it as a solvent such as for extraction, due to the fact hexane is profoundly neurotoxic, like it actually actively causes brain damage if you get exposed to enough. i had no idea until recently. one off isolated exposures are pretty harmless, but, god, routine exposure? its so bad for you, its not like say toluene where its just toxic but youll get over it, certain hexane exposures are accompanied by permanent loss of brain cells like they used to say what beer does.

Heptane and hexane are both chain molecules made of the same thing hence their very similar properties. its pretty common for heptane to replace hexane as a solvent.
Its scary to think how much brain damage has been caused by people hovering over their shellite as it evaporates down, the hazard has really been downplayed.
 
It is not easy to get heptane if you are a laymen in Europe. I found a product , Tikkurila RUISKUOHENNE 1032,a spray thinner which contains C7, the msds says it is 'technical heptane', so probably not lab-grade, but close.
SWIM had an extraction (STB) with this stuff, and had similar experiences/product like the thread starter. (small crystals, whitish colour).
However, SWIM had the problem, that for the first two round of freeze prep, the result was clear oil.
There might have been multiple mistakes SWIM made led to the oiling out: (probable causes - not sure)
  • not hot enough heptane at the very first extraction
  • instead of several smaller batch extraction, (like 7x30ml) , did it at once 210ml heptane
  • the raw material was in a form of very fine powder, and it did not spent enough time in the basic bath (only just an hour)
SWIM had to re-disolve the clear oil in hot naphta (benzinum -EC: 926-605-8, aka petroleum-ether 80/110) and then freeze-prep and finally let it evaporate.

1032 Thinner (see Product attachments)
EC number : 927-510-4 (Hydrocarbons, C7, n-alkanes,isoalkanes, cyclics)
 
mrstuff said:
It is not easy to get heptane if you are a laymen in Europe. I found a product , Tikkurila RUISKUOHENNE 1032,a spray thinner which contains C7, the msds says it is 'technical heptane', so probably not lab-grade, but close.
SWIM had an extraction (STB) with this stuff, and had similar experiences/product like the thread starter. (small crystals, whitish colour).
However, SWIM had the problem, that for the first two round of freeze prep, the result was clear oil.
There might have been multiple mistakes SWIM made led to the oiling out: (probable causes - not sure)
  • not hot enough heptane at the very first extraction
  • instead of several smaller batch extraction, (like 7x30ml) , did it at once 210ml heptane
  • the raw material was in a form of very fine powder, and it did not spent enough time in the basic bath (only just an hour)
SWIM had to re-disolve the clear oil in hot naphta (benzinum -EC: 926-605-8, aka petroleum-ether 80/110) and then freeze-prep and finally let it evaporate.

1032 Thinner (see Product attachments)
EC number : 927-510-4 (Hydrocarbons, C7, n-alkanes,isoalkanes, cyclics)
Click to expand...
Hi there, welcome and thanks for sharing!

Was your oily extraction, presumably, with MHRB?

An important matter of technique to consider is this: slower cooling leads to larger crystals. Too-rapid cooling will result in small crystals.

Oiliness may result from too high an initial concentration of DMT in the solvent, so heating the heptane may not help in this instance. Warm heptane anyway doesn't make much difference unless the base soup is also warm. Oiliness seems to crop up a bit more frequently at the moment, so I'm also wondering if this is down to specific batches of bark being (over?-)harvested at sub-optimal times. An hour of base contact time for finely powdered material should be perfectly adequate. All-in-all, tryptamines can have a tendency to oiling out sometimes.


One more thing I'm wondering is whether, somehow, that technical heptane has a slightly enhanced tendency to pick up moisture, and consequently whether a saturated brine wash of the pulls before freezing may have helped. However, seeing as the re-x from naphtha sorted it out for you, I also have a suspicion that it's the possible content of cyclics that led to the oiling.
 
It may seem a bit pedantic, but there is no such thing as "the best solvent". Recrystallization separates the desired compound from impurities, so the "best" solvent is the one the compound crystallizes "well" from (where "well" can mean rapidly, or fully, or something else you value) while the impurities remain dissolved (so the solvent choice depends on what impurities are there in the first place).

In the context of DMT extraction, heptane is often used, because of DMT's solubility profile in it. Some people add a tiny bit of ethyl acetate to boost solubility and deal with smaller solvent volumes.
 
Back
Top Bottom