Difference between revisions of "DMT Extraction Overview"

Revision as of 23:42, 19 May 2010

Note:

This section is a transcription of Entropymancer's DMT Extraction Overview[1]. The content is to remain accurate as such.

The following is not a Tek, but rather a concordance of Teks. Virtually all DMT extractions follow the same basic process; they differ only in whether the initial extract is acidified, and in what purification techniques they prefer. I posted it on another forum (the Shroomery), but figured it might be of use to some folks here.

The internet community has really stepped up in terms of providing step-by-step walkthroughs to guide the layman through the process of extracting DMT crystals. A quick search for DMT extraction teks turns up dozens of procedures; but how’s a body to know which tek to choose? I've seen a lot of posts by people having problems with purity due to trying to follow a tek too closely (especially ones that don't give the reader a target pH).

Really though, all of the teks out there boil down to the same process: Extract DMT into an aqueous solution, collect DMT as the freebase in a nonpolar solvent, then recover the freebase as a solid. All of the differences between teks are just differences in purification techniques. And depending on your starting material and available chemicals, the purification steps in any given tek may not suit your extraction. Which is why I've written the following extraction overview, so the extractor can chart a plan of attack that best suits their extracting conditions. I'm not going to go into mundane detail on accomplishing any particular step, just give enough information that someone acquainted with basic extraction processes could easily accomplish it. This level of detail is covered thoroughly in the teks.

Answer to the Most Frequently Asked Question Regarding DMT Extractions: Which tek do I use?

I know there are plenty of people who don't want to read all this, and just want to know what's the simplest tek to use. I've seen this question posted a million times, so I figured I'd include my answer in here, so I can link to it easily.

For anyone who doesn't wish to weigh the merits of all the methods, here is my recommendation: As long as you're extracting from Mimosa hostilis root bark, use Noman's tek or Marsofold's tek. But, instead of the ammonia wash of the final product, use the sodium carbonate wash from Vovin's tek (Step 7, pg 12). But be aware that a desire for simple answers may not serve you so well in your encounters with the spice.

1. Extraction of the Plant Material

Obviously the extractor has a fairly wide array of choices for a starting material to extract from (see the “DMT is Everywhere” chapter of TiHKAL), but the most popular choices are Mimosa and Acacia. If you are considering starting from some other material, you will want to think about the fat content of the material, and probably include more of the optional purification steps. Mimosa seems to be ideal, since many people report surprisingly pure product with minimal purification. Acacia is also a good option, although you will want to be certain to have at least one acid-base process in your procedure, either as the initial extraction or a later purification.

When it comes to the actual extraction from the plant material, there are essentially only two general processes to choose from:

• Acid/Base Extraction – Heat the plant material in water that has been acidified to pH 2-4 with your choice of acid to obtain a solution of the water soluble DMT salt. Hydrochloric, acetic, phosphoric, citric, and tartaric acids have all been used with good result. If you’re using any plant material other than Mimosa, it’s recommended that you follow this route because it lends itself to more thorough purification of the product.

• Straight to Base Extraction – This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. The basic idea is to simply cover the root bark with water basified to pH ~13 and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of hydroxide is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Sodium hydroxide is by far the most popular choice, though potassium hydroxide could be used instead. When going this route, a basic polar wash on your nonpolar solvent is practically a must; otherwise, some residual lye seems to remain in the product, making it more harsh. In the US, NaOH is a watched chemical due to its use in meth production. Ordering online or buying with a credit card could have undesired concsequences.

(Optional) First Defatting Opportunity (Acid/Base Extraction Only)

If you made an acidic extract of the DMT salt, you can now take the opportunity to remove unwanted plant fats and impurities by extracting your acidic solution with a couple volumes of nonpolar solvent and the solvent discarded. Naphtha, toluene, or xylene are all acceptable for this step.

2. Nonpolar Extraction of the Freebase

At this point it’s time to recover your DMT freebase into a nonpolar solvent. Xylene and toluene are not recommended for this step, particularly with Mimosa, as they will carry along a red pigment that can end up in your final product (some people extract with these solvents with the explicit intent of extracting the red pigment, which has been reported to be psychoactive itself). Naphtha is the most commonly used solvent for this step, but diethyl ether, methylene chloride (DCM) and hexanes have both been used successfully as well. Remember when extracting, you want to swirl or gently mix the layers, not shake them. Nasty emulsions can form, which are to be avoided at all costs.

• Acid/Base Extractors – Now you need to deprotonate your DMT back to the freebase. This is done by adjusting your acidic extract to pH > ~9.5 . Typically this is done by adding sodium hydroxide, but calcium carbonate or calcium hydroxide can also be used, depending on what pH you're aiming for. If necessary, the volume of the acidic solution may be reduced before basifying. The basic solution is then extracted with several volumes of nonpolar solvent and the extractions pooled. The basic solution now theoretically been stripped of DMT, and can be discarded. There is some debate over the optimal pH for this step. It's known that with certain plants sources (like Chacruna), a pH of 9 is sufficient to achieve maximum yields. On the other hand, Mimosa extractors have found that a much higher pH is necessary; this is likely due to the effects of various phytochemical solutes on the polarity of the aqueous phase. In theory, the addition of excess salt to the aqueous phase of a Mimosa extract prior to defatting ought to accomplish the same thing as the tremendous excess of hydroxide, but I've not yet heard of this being successful.

• Straight to Base Extractors – Your solution is already basic, so you’re good to go on this step. Just extract your basic, bark-filled mixture with several volumes of nonpolar solvent and pool the extracts.

(Optional) Acid/Base Purification and Defatting

If you did an acid/base extraction, this step is probably unnecessary, especially if you defatted before recovering the freebase. It can be done if you’re really worried about impurities and aren’t partial to any of the subsequent purification methods. If you went straight to base, then this step could be worth your while, as it allows you to defat your extract. On the other hand, many people find that Mimosa has little enough fat content that defatting leads to an unnecessary loss of product.

Extract your nonpolar DMT freebase solution with several volumes of water acidified to pH 3-4 with your choice of acid (hydrochloric, acetic, tartaric, etc.) and pool the extracts. If desired, defat the acidic solution with a couple volumes of nonpolar solvent (naphtha, toluene, etc.). Basify the solution to regenerate DMT freebase and recover by extracting with several volumes of extracting solvent (naphtha, DCM, hexanes, etc.), pooling the extracts.

(Optional) Washing the Nonpolar Solution

Many teks don’t include this process, which comes from Vovin's tek, but it seems to be the best option for those concerned about residual lye in the nonpolar phase. To neutralize any lye which still remains in your product, wash the nonpolar solution of freebase with a small volume of dilute sodium carbonate (washing soda), pH ~8.5 (this is not the same as baking soda, sodium bicarbonate). The layers separate easily without emulsion, so shake away, then drain the water from the bottom of your seperatory funnel (assuming you’re using naphtha so your organic layer is on top). Room temperature water should be used for the sodium carbonate solution to avoid cooling the naphtha and encouraging precipitation. If desired, you can perform a couple more quick washes with neutral (unbasified) water to remove any traces of the sodium carbonate which may have been left in the naphtha.

3. Recovering the DMT Freebase from Solvent

There are basically two schools of thought on this step: evaporate the solvent or precipitate DMT crystals by freezing. There’s nothing really wrong with simply evaporating if you’re going to be doing further purification on the material, but that being said, I still don’t really see any reason to do it until you’ve freeze-precipitated a majority of your product.

To freeze precipitate, put your nonpolar solvent in the freezer (with the temperature setting as cold as it will go), and allow it to sit overnight. Depending on how concentrated the solution is, a good portion of DMT ought to precipitate out as nice crystals. These crystals can be removed but must be dried quickly or in a cold environment, because they will redissolve as the solvent warms up. At this point your best bet is probably to reduce the nonpolar solution to something less than half its original volume, and freeze precipitate again. Repeat until no crystals result or the crystals have significant visible impurities, at which point you can either discard the remaining mess, or evaporate the nonpolar solvent and recover the last shreds of DMT by further purification. In a simple variation on freeze precipitation, some people report success in growing larger crystals by repeatedly transferring the recrystallizing solution back and forth between the freezer and fridge every few hours.

Now the only thing left to do is purify the loot.

(Optional) Wash Crystals with Cold Aqueous Ammonia (Not Recommended!!!)

This is a simple way to wash out some minor impurities and discoloration. Just set up a filtration apparatus, put the crude DMT on the filter, and rinse with a small volume of ice-cold aqueous ammonia (preferably 10% concentration). Many people have run into problem with this method, resulting in the ammonia dissolving away their product, making it difficult to recover.

(Optional) Recrystallize from Hot Solvent

This will help to reduce impurities and give the product a more sharply defined melting point, but it won’t do much to reduce discoloration unless combined with activated charcoal (see below). To recrystallize, dissolve your product in a minimal volume of hot solvent (e.g. roughly 20 mL naphtha per gram of DMT) and allow the solution to cool slowly with minimal agitation. Once it has reached room temperature, transfer it to the fridge for a couple hours, then to the freezer. Though it’s not necessary, if you have a small DMT crystal on hand, you can add it to the solution to help seed the recrystallization. Regardless, a nice crop of crystals should precipitate out of solution, and can now be collected by filtration. If unsatisfied with the results of a recrystallization, you can always reheat the solvent to redissolve the DMT and reduce the solution volume, then repeat the cooling process. Naphtha is the most commonly used recrystallization solvent, but success has also been reported with hexane.

(Optional) Clean with Activated Charcoal

This seems to be the most effective and reliable method for removing discoloration. Proceed exactly as though you were recrystallizing, but after dissolving the DMT in hot solvent, add a small quantity of crushed activated charcoal and swirl occasionally, sustaining heat for about ten minutes. Decant the hot solvent from the charcoal and allow to crystallize as usual. This method generally removes only discoloration-related impurities and requires a fairly clean starting, which is why I don’t recommend doing it with the crude nonpolar freebase solution prior to the initial freeze-precipitation.

(Optional) Acid/Base Purification and Defatting

Unless your extraction was extremely messy and gave you a gunky mess instead of crystals, then this step is total overkill. If your product is a roughly crystalline solid, a wash with cold aqueous ammonia and recrystallization with activated charcoal treatment should clean it up just fine. But if you want to recover any DMT from the gunk you get evaporating your solvent after freeze-precipitating, this is the way to do it. Take up the crude material in water adjust to pH 3-4 with your choice of acid. Defat if desired, then basify, extract, and precipitate.

(Optional) Purify by Column Chromatography

Obviously this route is not for the average extractor, and assumes you have access to a chromatography column, or at least a buret which can function the same on a smaller scale. It is totally unnecessary unless you're aiming for analytic purity or you have a godawful extraction goo that calls for some heavy-duty purification. You may run a TLC first using the same solvent pair that you plan to run the column with to get an idea what you'll be up against, but this is probably not necessary. The DMT can be visiualized under UV light as a blue spot.

Plug the stopcock end of your buret or column with a glass wool (or less ideally, cotton) filter. Cover this with a small portion of sand and fill your column with silica slurry. Load your crude sample, and elute with your chosen solvent pair. Monitor the progress of the DMT with a UV light to capture the correct fraction. If you don't understand what any of this means, you probably shouldn't attempt it, but you can consult a lab manual to satisfy your curiosity.

Reference

1. ↑ DMT Extraction Overview[1]