I've been browsing the nexus recently again, having joined in 2012 for my first venture into DMT, after which I took a long hiatus. However, I've played around with several extractions over the past week and a half. I've been very greatful for nexus members who have done much of the experimental legwork for me, allowing me to mix-and-match for the most part to rapidly arrive at a protocol which for my purposes seems ideal. This has allowed my recent DMT project to arrive at fruition much more quickly than similar projects that arise in my professional and personal life. With that in mind, I thought I'd share my experiences, which might be useful for someone with similar inclinations and resources, or just for those who are curious.
To begin with, I'll state my aims and limitations.
I have very limited time, and I also wanted to avoid scheduling something that would need attention over several days, since my schedule is variable.
I also do not regularly consume DMT, so I wanted it to be pure. I don't care too much about yield though, as long as it is within reasonable limits. I also don't care about beautiful crystals.
I dislike filtering liquid for solid product, since I think it is messy and inefficient.
I dislike freeze - recrystallization because it involves waiting and isn't 100% efficient. I also just hate scraping crystals in general out of a jar; I much prefer to razor them off of a flat surface.
I also wanted to avoid multiple pulls of anything, since this seemed to be time-inefficient as well.
Finally, I wanted to avoid any distillation or chromatography, since this takes time to set up.
With this in mind, I found the following protocol to be a rapid way to create fully consumable product in 4.5-6 hours.
A 1 L bottle is filled with 50 - 250 g powdered ACRB. Water is added so that the hydrated plant material, once expanded and settled, is roughly two centimeters under the surface of the liquid.
The pH of the slurry is adjusted to 2.5 with 12.1 M HCl, adding slowly to allow the concentrated acid to diffuse and avoid destroying alkaloids on contact [not sure if that would happen at any appreciable rate, but I figured I might as well avoid it]. The mixture is then sonicated in a bath sonicator for 30 min.
After sonication, the slurry is divided into 50 mL conical tubes and spun down at ≥6000 rpm for 10 min. During this time, the original sonication bottle is rinsed, dried, and fitted with a funnel and a 200 mesh (75 micron) stainless steel screen. The supernatants are decanted through the screen, and the large pellets are discarded. The volume of liquid is decreased considerably at this point, by up to 35%, having been absorbed by the centrifuged pellets. Next, the liquid is passed into a new bottle through a 0.22 micron bottle top filter under vacuum pressure, removing any particulate matter that may trigger the formation of emulsions during liquid-liquid extraction.
The solution is then basified with a 6 M NaOH solution to pH 13. 20% v/v dichloromethane is added. The bottle is stirred for 30 min (covered, without heat), then allowed to settle until it has formed a neat phase separation, typically about 20 min. The basic aqueous portion on top is decanted most of the way (~80%) into one of the used bottles, then the remainder of the liquid-liquid mixture is added to a separatory funnel. After separating and discarding the initial aqueous portion, the dichloromethane is washed once with a 30% v/v aqueous solution of 0.1 M sodium carbonate and between one to three more times, 20% v/v, with an aqueous brine solution. Before the last wash, the separatory funnel is rinsed with water, acetonitrile, and water again to ensure that it is fully clean and dry.
Next, FASA is added slowly to the flask with a 10 mL serological pipette. With the larger preparations, it quickly becomes impossible to see if any more product is precipitating after a few mL of FASA. [Early on, I would typically wait until the precipitate settled to keep adding more, but now that I am relatively familiar with my plant material, I usually add all the FASA I plan to in one step.] Once no more product precipitates after FASA addition, water is added slowly to the mixture while it is being stirred until all the precipitate disappears again. This new mixture has three solvents but only two layers, since water and acetone are highly miscible. The dichloromethane is drained onto a small pyrex plate, and the water/acetone mixture is drained onto a large one. Both of these are placed in a fume hood to dry. If discipline has been used in adding FASA and water slowly, there should be little solvent left. The dichloromethane is evaporated mostly to see if any freebase was left after the FASA addition. In my working conditions, evaporation usually takes less than two hours, bringing us from start to finish in under five hours if you’re happy with fumarate.
While I enjoy the fumarate orally, most others I know prefer the freebase. I’ve done several different things from this point on to accommodate this: heptane recrystallization, heptane evaporation, water recrystallization, carbonate-fumarate paste, and even dichloromethane evaporation. The paste method works well for me, as does DCM evap. Both of these take less than one hour under air. Not surprisingly, the recrystallization techniques get the best crystals, but for me usually have had the lowest yields, at least in any reasonable amount of time.
My yield with this method has been coming out to around 0.8-1.2%.
Below are some of my nicer crystals under a microscope. These were created using RP-HPLC, just to see if there was something wrong with my raw material (I was extracting goo at first). Hard to believe ACRB can give such nice ones based on some of my earlier extraction attempts.
fredkern attached the following image(s):
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