Chilled Acetone with IPA and Naphtha

CIELO

Introduction

CIELO stands for Crystals In Ethyl-acetate Leisurely OTC (Over The Counter).

In this TEK, aqueous alkaline cactus paste is extracted with chilled ethyl acetate. The extract is salted with excess citric acid to force the precipitation of mescaline citrate crystals directly in the solvent.

This process was developed in a loving collaboration at the DMT nexus. Deep thanks and gratitude to everyone who contributed or provided support: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Loveall, and others.

Safety

Review ethyl acetate's safety information and check the manufacture's MSDS to verify you have pure ethyl acetate. Make sure any plastic you use is compatible with ethyl acetate and verify your ethyl acetate evaporates cleanly.

Following this advice does not guarantee safety. It is up to each adult individual to make their own decision on proceeding with this process.

Materials

• Food scale (gram resolution)
• 300g water
• 25g lime
• 32 oz jar or french press
• 100g powdered cactus (outer skin)
• ~1000g chilled (freezer ~ 0F) ethyl acetate† (sometimes found as "MEK Substitute")
• Large jar (e.g. 64 oz)
• Coffee filters, filter support, and jar funnel
• 5g of citric acid
• Small storage jar
• Jeweler scale (mg resolution)

Fig. 1: Materials used in the CIELO Tek.

Process

Paste

Mix water and lime in a ~32 oz jar or french press) to make milk of lime. Incorporate cactus while stirring and continue stirring for at least 10 minutes to a smooth paste. Allow paste to react for 24 hours and mix again for a few minutes.

Fig. 2: Reacted alkali cactus paste ready for extraction with chilled ethyl acetate.

Pull

Add ~ 300g of freezer chilled ethyl acetate (~0 F) to the paste, mix for 60 seconds, and decant/filter to a large jar (64 oz). If using a french press squeeze very gently to avoid pulling water. Immediately pull 5 more times with ~150g of ethyl acetate stirring for 60 seconds each time. Final extract should be clear with no droplets or particles (see Fig. 3).

Fig. 3: Clear extract from cactus paste using chilled ethyl acetate. No particles or droplets are present.

Salt

Verify no particles or droplets are in the extract. If any are present, decant/filter to remove them.

Dissolve ~ 5g of citric acid into extract. Solution will become cloudy (Fig. 4) and crystals will form after some time (Fig. 5). Move extract to the fridge overnight to complete crystalization and swirl to remove crystals from the wall (Fig. 6).

Fig. 4: Cloudy extract after citric acid addition.

Fig. 5: After some time mescaline citrate crystals begin to form.

Fig. 6: After spending the night in the fridge and swirling, mescaline citrate crystals accumulate at the bottom.

Finish

Catch crystals in a coffee filter. Rinse jar with a small amount of fresh ethyl acetate to pickup any remaining crystals in the jar and wash crystals in the filter . Repeat this about two more times until green color is removed and all crystals are in the filter. Allow crystals to dry and collect. This is the final product (Fig. 7).

Mass spectrometry (MS) results from solaris analytical indicate the product is very clean mescaline (Fig. 8). In this examples the yield for mescaline sulfate was 1.4%. Depending on the starting material and technique, the yield range is usually 0.2% to 2%

Fig. 7: Final product.

Fig. 8: Mass spectrometry result. Peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are mescaline with amine/methyl/methoxy groups cleaved giving the lower mass spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline.

Appendix: Development Notes

What worked

Chilled ethyl acetate was found to make the process robust experimentally, presumably by minimizing water and plant material while remaining efficient for pulling mescaline. By using chilled solvent users are less susceptible to cactus plant variability.

It is also possible to obtain good results with 3 minute room temperature pulls, but the results may not be as consistent between users as with chilled ethyl acetate. Sometimes it can take longer for crystals to form, while other times crystalization can be very quick when using a magnetic stirrer. With room temperature solvent 5mg/g of citric acid can be enough when working with outer cactus skin, but not when working with the whole plant.

What didn't work

Paste modifications: No improvements seen with microwaving, partially drying, adding NaCl, or extending the reaction time beyond 24h. Completely drying the paste made the process not work, apparently some water is needed in this process.

Pull modifications: Long room temperature pulls made the paste congeal and resulted in lower yield. Heating during the pull did not improve yields. In general the crystalization is more difficult and the product can aquire a tan color if the pulls are more aggressive with no improvement to yield.

Extract modifications: Chemically drying the extract with a drying agent such as anhydrous MgSO4 before salting had no yield benefit. In one example, drying the extract with CaCl2 resulted in a more difficult crystalization and a 40% yield loss. In general, any water content in ethyl acetate directly from the pulls is already in a good range experimentally.

Note: Droplets or debris not decanted/filtered before salting may result in poor crystalization. It is very important to verify the extract is free of these issues before salting.

Salting and crystalization details

During salting, every 10mg of citric acid (H3Cit) reacts with free base mescaline (Mes) to form to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):

3Mes_(↑) + H3Cit_(↑) ⇒ 3(MesH)Cit_(↓)

The TEK calls for ~twice of what am outlier like the legendary Ogun cactus would need (~1100mg of citric acid for 100g at 4.7% yield), and ~8 times what the average cactus would need. The reason is that excess citric acid induces crystalization to overcome any water or plant material that would otherwise keep mescaline citrate in solution. This is a simple but very important lab observation, compatible with Le Chatelier's principle. There is a lot room for excess citric acid in ethyl acetate since its solubility is 50mg/g (and water in the solvent from the pulls may increase this solubility further). The TEK recommends 2mg/g since this was found to be enough to crash mescaline for most users when using chilled ethyl acetate, but others may need more citric acid because of cactus differences (e.g. outer skin vs hole, different species, growing condition, etc) or TEK execution variability (warmer solvent, longer pulls, etc).

Finally, other solid organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested. Sulfuric acid, HCl, and phosphoric acids could be investigated (and crystals have been observed after adding sulfuric acid to the extract). However, these stronger acids may interact with ethyl acetate or cause water droplets issues.

Disclaimer

It is possible that some of the assumptions and conclusions in these lab notes are incorrect or incomplete. The process was tested in several ways, but the search was not exhaustive. There could be ways to improve this process.