Latest revision as of 07:02, 4 July 2022

Introduction

This Tek was created by Brennendes Wasser.

Thanks to everyone who has contributed or helped experiment to aid in refining/ improving this process:

This Tek is more or less completed. Lab and test results have been confirmed and are very promising. Feel free to contribute. More photo's to follow soon.

Please take your time with your first extraction, although this is an easy Tek you don't want to rush it and make a mistake.

Forum Link[1]

Safety

Review Acetone ^[1] ethyl acetate^[2] and citric acid^[3] safety information. Verify solvent MSDS, plastic compatibility, and clean evaporation.

This TEK is food safe if food grade materials are used.

Following this advice does not guarantee safety. It is up to each adult individual to make their own personal decisions.

Consumables

100g of anadenanthera peregrina seeds or Anadenanthera colubrina
25g Sodium Carboante/ additional 1.85g for later
150ml water (spray bottle)
25ml Water for later
450ml Naphtha
450ml Acetone or alternatively 450 Ethyl Acetate
3g of citric acid or furmaric acid
Sodium Carbonate
Jars
Coffee filter, lab filter or cotton balls (with funnel)
3x 100ml 1:3 Ethyl Acetate:Naphtha

Equipment

Blender
Kitchen scale
Coffee filters, support basket, and funnel Or lab filter and vacuum pump.
Glass jars with lids
Fridge
Milligram scale
Spray Bottle
Fry Pan and stove

Detailed Process

Heat Seeds

-Place seeds on minimal heat on fry pan, bring it up to heat until they start popping, lower the heat and turn it off once the seeds have stopped popping.

Powder

-Get 100g seeds and 25g of sodium carbonate grind them with a glass blender into a powder. (Check weight on scales and take note).

Add water

-Add 150ml of water by spraying the seeds/ sodium carbonate mix with a spray bottle. Do this until the paste becomes doughy. Mix well.

Dry Paste

-Dry the paste with a fan and optionally low heat.

Defatting

When dry (check by comparing weight previously noted), defat with 3 x 150 ml boiling Naphtha, then decant.

Pull

Extract and pull with 3 x 150 ml DRY Acetone, filter. Alternatively Ethyl Acetate can be used and may be a better option.

Boiling the solvent should increase solubility so a hot water bath is recommended (no open flames near solvent). You should be using glass jars, ensure glass containers have lids to minimize evaporation of solvent.

Salting

-Add Fumaric acid or citric acid at least 3 g, slowly, then stir vigorously. Let it rest for 12 h, then decant and watch if the Acetone precipitates more, also check if adding more FASA causes further clouding and let the Alkaloid-Fumarate crystals dry off any remaining Acetone. Note using citric acid may negate the need to wait 12h.

Decant

-Decant Acetone (or Ethyl Acetate if using that)

Dissolve Goo

- Dissolve the Alkaloid-Fumarate crystals (or citrate) in 25 ml hot water. Slowly pour another a solution of 1,85 g Na2CO3 (0,5:1 Na2CO3:Alkaloid-Fumarates) in 25 ml water. This will form impure freebase bufotenine (either as a blob or crystal if you defatted adequately enough). Decant water.

If the ratio's are off and a blob or crystals do not form you can evaporate the water with the freebase still in it and proceed to next step. You will be left with a mix 'dry' of freebase alkaloids and sodium carbonate. Proceed to the next step and pull with EA/Naphtha.

Note if you evap results will be more impure.

Base

-Extract the brown precipitating freebase alkaloid blob with 100 ml portions of 1:3 Ethyl Acetate:Naphtha. Do this until the freebase blob does not shrink anymore. Black powder will remain. Dont combine the pulls, but put them in the fridge separately. The freebase blob may solidify to a ball upon stirring within this process. Break it apart, if it becomes hard, to speed up extraction. If it remains a goo, still just proceed extracting. Place decanted solvent mix from each pull in the fridge for fridge-frecipitation.

Alternatively (Experimental still-but works well): One can do a few pulls with ethyl acetate only and then place it in a small glass dish with xylene 1:3 ratio (amount still being confirmed). And start to evaporate it.

So the idea here is to pull the freebase bufotenine with EA (EA may pick up some impurities) and place it with xylene. Bufotenine wont dissolve in room temp xylene (or even heated bufotenine <139 celcius).

Since EA boils at 70 degrees and xylene at 140 degrees celcius, the idea is to let half the EA/ Xylene mix evaporate. At this point majority if not all the EA should have evaporated out leaving behind xylene only. Xylene won't hold bufotenine freebase so it crashes out as a white residue/ crystal. The majority of the impurities stay in the xylene as it is quite a large spectrum solvent. Once the bufotenine crashes out one can decant the xylene and dry the dish for bufo crystals. Crystals will be white but as you scrape it up it may become slightly brown (it will sometimes stay as white crystals). The browning that can occur is believed to do with over evaporating the xylene, xylene and EA ratios, and or depends on how well the de-fatting was performed.

Keep decanted xylene for the next run/ extraction, it may contain tiny amounts of EA and therefore bufo.

Note: The alternative method is safer than boiling xylene and may pull more efficiently than EA/Naphtha mix. Note MS-LC data on this method has not be compiled.

Crash/ Filter TEK Complete

Collect your precipitated freebase Bufotenine (decant solvent). The solvent mix itself will still contain Bufotenine. Evaporate the rest to get all the remaining Bufotenine with a slightly lower purity.

Bufotenine yield: 1-3 % to seed weight This is very pure bufotenine 96%+ purity/

Bufotenin recrystalization (optional)

Bufotenin recrystalization for 99.99% purity

The best solvent to form crystaline Bufotenin is Xylene. Actually it would be way too unpolar to ever dissolve Bufotenine. As you can heat Xylene above the melting point of Bufotenin, the latter suddenly becomes soluble while liquifying, while the more polar 2 % dark impurities will remain undissolved. This way you can create 100 % purity Bufotenin from 98 % purity Bufotenin retrieved by the former mixture. See the following :

1 = Break up crude Bufotenine chunks (if even solid) 2 = Heat in Xylene > 140 °C until only brown powder is leftover (see solubility table how much to use) 3 = transfer surfactant Xylene into new Jar and let it sit until surfactant is clear 4 = dry crystaline Bufotenine - much faster if you wash it with low-boiling Naphtha

Note the fumes are highly dangerous for your health and combustible. You should use the required PPE and have very good ventilation (as in outdoors).

Lab Analysis

Not much to say, all the signals are there (and the big Methyl signal is indeed like DMT of course, not like the wrong simulation). As it is measured in MeOD you can see 2 big solvent peaks. These are marked red, so you can just ignore them. Also there are traces of EA present. The only unidentified peaks are marked gray and these are just traces. In total their integral is just 0,30 and the peak fraction of Bufotenine derived from this number is 97,87 %. Now this does not automatically translate into a purity of 97,87 %, but I may say that still the purity is somewhere between 96 - 99 %.

Further investigations

-Sodium Carbonate is the only base you should use do not use calcium hydroxide or caustic soda/lye.

-Drying the product in the microwave has been tested to a limited compacity and should work.

-Furmaric or citric acid should work and have been successfully tested.

-Ethyl acetate instead of acetone for the initial pull should work.

-Warming the EA or acetone for the first pull should increase yield.

Reuse

Reusing solvents is encouraged^[4] at the DMT nexus.

Wash spent extract with sodium carbonate saturated water (35% by weight). About 1/5 of the solvent volume as saturated water is enough. Shake vigorously (emulsions do not form). CO2 bubbles may be visible during citric acid neutralization. Keep an eye on any bubbles and release any pressure buildup regularly. Neutralization can be optionally verified with pH paper. Rest washed solution until clear (up to a day or more).

Remove the water layer with a pipette or separatory funnel. Freezing the solvent and filtering the ice slush that forms with a metal strainer is also an option. Finally, decant off any excess solid sodium carbonate/citrate. CaCl2 (sold as deicer, calcium hardener for pools and sometimes is the only ingredient in moisture absorbers tubs) can be used to ensure there is no water still left in the EA.

References

Ethyl Acetate Safety[2] Citric Acid Safety [3] Reusing Solvent [4]

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@@ Line 94: / Line 94: @@
 <font color="green">  Alternatively (Experimental still-but works well):
-One can do a few pulls with Ethyl Acetate and then place it in a small glass dish with xylene 1:3 ratio (amount still being confirmed). And start to evaporate it.
+One can do a few pulls with ethyl acetate only and then place it in a small glass dish with xylene 1:3 ratio (amount still being confirmed). And start to evaporate it.
 So the idea here is to pull the freebase bufotenine with EA (EA may pick up some impurities) and place it with xylene. Bufotenine wont dissolve in room temp xylene (or even heated bufotenine <139 celcius).

Difference between revisions of "BW's Bufotenine Dry Tek"