Kitchen Chemistry - Extraction and Synthesis

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Kitchen Chemistry Some good things to know

-------------------------------------------------------------------------------written by Black Peter (with invaluable help by Bilbo) distributed by the Visionary Plants List additional formatting by Andrew Edmond and Dave Gross Preface: I want to preface this with what I see as the advantage of the home cultivation of legal entheogens and the extraction of the aforementioned in the kitchen (or any room of the house, for that matter). First and foremost, there is the peace of mind in not having to buy illegal substances. Secondly, there is the magical feeling of having at your disposal a means of altering consciousness; when you cultivate these plants, the state has been through a long consecration of sorts while you tended to the plant bearing the particular "spirit." If you keep everything in it's proper place, should you be afraid? Why don't you cultivate yet something different altogether in conjunction with your plants to justify your owning owning the solvents needed? needed? One could begin painting, wine making, making, or anything else constructive and healing. Remember it's been claimed that those who live happy lives and develop their potential have the inertia of the universe to help them. I want to briefly touch upon the entheogens as they exist in the less technological area of existance. It is conjectured that the Kykeon of the Eleusian Mysteries contained none other than Ergine (LA-111), it's source being Claviceps purpurea (ergot). Albert Hofmann guessed that a water-based extraction from ergot infested barley would have isolated the LA-111 and left behind those substances responsible for the horrific phenomenenon phenomenenon known as ergotism. Ergine has been present in other cultures and has been present in other plant sources. Morning Glory seeds and Baby Hawaiian Woodrose seeds contain LA-111; Baby Hawaiian Woodrose seeds contain .3%. LA-111 is the active principle of the Ololiuhqui ("rounded things") of the Aztecs. Among the entheogens that man has used ritually is Cannabis sativa (Cannabis indica is actually a subspecies of this according to Ott), N,N-Dimethyltryptamine N,N-Dimethyltryptamine in various plants, beta-carbolines, 3,4,5trimethoxyphenethylamine trimethoxyphenethylamine (mescaline), muscimol/ibotenic acid, psilocin, and many others. My first rather grandiose claim of having this revised by actual chemists never saw the light, due to time constraints; the university can be a very hectic place, especially to an undergraduate. This is, however, a public work; feel free to revise and add to it if you will. If it is revised, please make a note of it and file:///C|/My%20Shared%20Folder/Books%20&%20Essays/...20-%20Extraction%20and%20synthesis%20of%20drugs.txt (1 of 9)3/31/2004 11:26:40 PM


change the version number.

-------------------------------------------------------------------------------Contents: What is the basic theory behind this? Alkaloids pH Polarity Reflux/Soxhlet Extraction/Washing What are some more technical things? Merck Index What are some tools that I will need? What are some conversions that I can use? How do I determine the alkaloid content of my plant material in milligrams? What are some clever home versions of lab equipment? Reflux Apparatus Soxhlet Apparatus What are some good algorithms? DMT Mescaline THC Psilocin LSAs Harmaline -------------------------------------------------------------------------------What is the basic theory behind all this? Alkaloids First of all, this is refering to extractions and not synthesis. We will not be creating; we will be extracting what nature has already created. For the most part, we will be dealing with alkaloids. The word alkaloid means "alkaline-like" and refers to a substance existing in a plant that contains nitrogen and exerts an effect on animal life. The former is something that you probably will never have to remember and the latter is important for obvious reasons. The important thing to know is whether or not the substance that you wish to extract is an alkaloid or not. The reason is that if it is an alkaloid, it will share some universal properties with other alkaloids that make it possible to create methods that apply to any plant source, depending more upon the matrix that the alkaloid is contained in than anything else.

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The only exception to this following of universal rules is mescaline, which will be expounded upon when it comes time to discuss it's extraction. Almost every psychoactive agent known at this time is an alkaloid. As the etymology of the word implies, alkaloids exist in a natural form that is above pH 7. An alkaloid exists in this basic state and is not soluble (dissolvable) in water that has not been acidified. It is soluble in an alcohol. When the pH is changed to acidic, the alkaloids will dissolve in water in a salt form.

-------------------------------------------------------------------------------pH The hydrogen ion concentration is known as the pH. There may be other explanations, but we shall not concern ourselves with it here. The scale is from 1 - 14, where the strongest acid is 1, neutral is 7, and the strongest base is 14. As mentioned before, the alkaloid will dissolve in water when the pH is acidic. What happens is that the combination of an acid and a base forms a water-soluble salt. When the solution is basified, the alkaloids are no longer in salt form, and are then soluble in a non-polar solvent. REMEMBER: ACID + BASE = WATER SOLUBLE SALT iff (if and only if) pH < 7 ACID + BASE = NON-POLAR MOLECULE (freebase) iff pH > 7

-------------------------------------------------------------------------------Polarity The polarity of a molecule is, for non-chemists, whether or not it will dissolve in water. If it is polar, then it will dissolve in water and if it is non-polar, then it will not. Actually, polarity refers to a situation on the atomic level where net electrical charges are unbalanced. REMEMBER: LIKE DISSOLVES IN LIKE. The polarity of the solute and the polarity of the solvent must be the same. A solution consists of a solvent and a solute.

-------------------------------------------------------------------------------Reflux/Soxhlet: To reflux is to use a reaction solvent to keep a material dissolved and at a constant temperature by boiling a solvent, condensing it, and returning it to the vessel. Soxhleting involves this same process except for the fact that the material is separated from the solvent. It's much like percolating coffee.

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Extraction/Washing: Washing involves the separation of impurities from a pure source and extraction involves the separation of purities (forgive my play on words - it's a memory device) from an impure source. Look at the algorithm for LSA's; the first part is a washing and the second part is an extraction. For an extraction, you need two liquids that are insoluble in each other. That means that they will form two visible layers. An example is home-made salad oil; the oil floats on top of the water. The most technical thing that we will need is pH paper - chemists use a sep funnel; we will use a turkey baster.

-------------------------------------------------------------------------------What are some more technical things? Merck Index: A reference book of chemicals, mostly drugs. I will give the listing for our friend DMT followed by an explanation. 3259. N, N-Dimethyltryptamine. N,N-Dimethyl-1H-indole-3-ethanamine; 3-[2-(dimethylamino)ethyl] indole; DMT. C12H16N2; mol wt 188.26. C 76.55%, H 8.57%, N 14.88%. Occurs naturally in plants with hallucinogenic properties. Isoln from the leaves of Prestonia amazonica (Benth.) Macbride (Haemadictyon amazonicum Spruce & Benth.), Apocynaceae: Hockstein, Paradies, J. Am. Chem. Soc. 79, 5735 (1957). Synthesis: Szara, Experientia 12, 441 (1956) using the method of Speeter, Anthony, J. Am. Chem. Soc. 76, 6209 (1954). Relationship between hallucinogenic activity and electronic configuration: Snyder, Merril, Proc. Nat. Acad. Sci. USA 54, 258 (1965). H / \ / N \ | |_____| \ / \CH CH N(CH ) 2 2 32 Crystals, mp 44.6-46.8*. pKa 8.68 (ethanol-water). Freely sol in dil acetic and dil mineral acids. Picrate, mp 169.5-170* Methiodide, mp 216-217* Caution: May produce serious psychologic disturbances. 3259 is the compound number. C 76.55%... is elemental analysis data; the percent of each element in the compound. References to journal articles comes after this, followed by a structural formula. Lastly is melting point and solubility data. -------------------------------------------------------------------------------What are some tools that I will need? A Pyrex baking dish - this is a glass container that is used for cooking in the mainstream world. We will file:///C|/My%20Shared%20Folder/Books%20&%20Essays/...20-%20Extraction%20and%20synthesis%20of%20drugs.txt (4 of 9)3/31/2004 11:26:40 PM


be using it for evaporation. A turkey baster - this is used as a siphon. It is in lieu of a separatory funnel. A layer is generally removed from a solution with the turkey baster and eventually evaporated in the Pyrex dish. A glass measuring cup with metric conversions. A blender, coffee grinder or spice mill, or both - This is to thoroughly grind the plant material as finely as possible. A centrifuge juicer - this is for use with mescaline containing cactii. The cactus is put into the centrifuge juicer, the pulp is then removed and mixed with lemon or lime juice, and then placed back into the juicer. A slow cooker ("Crock Pot") - this is used in preparing ayahuasca that will be taken orally. It is also used in heating the plant material in an acidic solution in lieu of alcohol soaking. It is, in theory, faster. Lemon juice, lime juice, or vinegar - this will be used in several methods involving the separation of the alkaloids from the solid plant material. Alcohol - do not use Isopropyl alcohol. You will need either ethanol (grain alcohol - sold as "Everclear"), methanol (sold as Wood Alcohol), or denatured alcohol that has methanol as it's denaturant. This last one should be only when you cannot find either of the other two. Ethanol, as you probably know, can be ingested. The latter two are highly poisonous and must be evaporated until there is no more smell (not simply until the surface appears dry). Lye - a nasty creature to work with. It is extremely dangerous as it behaves ironically like you would think an acid would behave after watching old movies. It is a strong base. A brand name is "Red Devil Lye". Keep in mind that when water is added, it bubbles, releases some very caustic fumes, and heats the vessel that it is in tremendously. So obviously, do not shake some in a jar with a lid on it to mix. After it has bubbled, then it can be added to a solution and that jar can be shaken. A Non-Polar Solvent - I once believed that Naptha is good. It is in 3 forms that I know of: Zippo Lighter Fluid, Energine Spot Remover, and in generic forms in any hardware store. The first two can be found in a grocery store but are much more expensive. The best non-polar solvent is probably white gas Coleman's Lantern Fuel. It is only a few dollars a gallon and supposedly is the cleanest. I can only guess that Naptha can be cleaned with a "speed junkie" algorithm used in making pseudo methamphetamine (the one with the Vick's inhalers). This may not be a sound idea, but here it is anyway for reference. A quantity of (in this case) naptha is put into a jar with the same amount of water, the jar is shaken vigorously for 5 minutes (the method calls for an aspirin bottle) and the top layer is siphoned off with an eye dropper or turkey baster. Be sure to vent the jar. Jars of various sizes. Coffee filters and thick paper towels - for filtration. Solutions containing lemon juice cannot penetrate a coffee filter so paper towels must be used. Cheesecloth is supposed to be good also. pH Paper - can be found in winemakers' catalogs. Gelatin capsules - found in health food stores. A Candy Thermometer - found in any grocery store. I am hoping to find a way to use this to manipulate some of the treasures hidden in poisons (ibotenic acid/muscimol, etc... ) -------------------------------------------------------------------------------What are some conversions that I can use? file:///C|/My%20Shared%20Folder/Books%20&%20Essays/...20-%20Extraction%20and%20synthesis%20of%20drugs.txt (5 of 9)3/31/2004 11:26:40 PM


1 cup = 250 ml 1 tablespoon = 3 teaspoons = 15 ml 1 teaspoon = 5 ml F = 9/5 C + 32 Avoirdupois 1 pound = 16 ounces or 1 ounce = 28.349 grams * Avoirdupois refers to a system where a pound equals 16 ounces -------------------------------------------------------------------------------How do I determine the alkaloid content of my plant material in milligrams? When I see something like "such an such plant contains .36 % DMT by weight," how does this benefit me? Well, all one needs to do is this: Figure out the number of milligrams per gram of plant material, and go from there. All you need to do is move the decimal one place to the right and you have the number of milligrams per gram of plant material. For instance, plant X has .30% DMT. I wish to take 60 mg, so I will need to extract from 20 grams of plant material. The reason is thus: per cent means "divided by 100" (all in all) and milli means "one-thousanth" (3 decimal places). Divided by 100, you move 2 decimal places to the left, multiplied by 1000, you move 3 to the right.

-------------------------------------------------------------------------------What are some clever home versions of lab equipment? Reflux Apparatus: What is needed is a small pot, a large stew pot with a lid that is at least 50% wider and twice as deep, a large metal tub that is at least twice as wide as the stew pot, an electric hotplate with 2 burners, several yards of 1 inch rope, 3 millimeter thick trash bags, an innertube cut into 1 inch thick rubber bands, and a large bag of ice. The tub is placed on the hotplate, the rope is curled in the tub with the large pot resting on top of it preventing the pot from directly touching the tub. The small pot containing the powdered material and solvent is placed in the stew pot; the stew pot has it's lid upside down. A piece of the plastic bag is cut and placed over the lid of the large pot so that it extends halfway down the side. Two large innertube rubber bands secure the plastic sheets. These are positioned several inches down the side of the pot, allowing slack in the plastic sheeting. Any air that is trapped under the plastic is forced out by loosening the rubber bands and flattening the bag with the hand. As much ice as possible is placed on top of the plastic covered lid. The tub is filled half way with water which is brought to a boil. This heats the apparatus to about 212 F, but not above. REMEMBER TO ALWAYS COOL THE APPARATUS COMPLETELY WHEN REFLUXING AND SOXHLETING BEFORE DISASSEMBLING BY POURING ICE INTO THE TUB! The Solvents used: file:///C|/My%20Shared%20Folder/Books%20&%20Essays/...20-%20Extraction%20and%20synthesis%20of%20drugs.txt (6 of 9)3/31/2004 11:26:40 PM


Methanol or Isopropyl alcohol - yeilds a product half as potent with Cannabis* or Ethanol or Petroleum ether - yields a product twice as potent with Cannabis* *Compared to ethanol/methanol -------------------------------------------------------------------------------Soxhlet Apparatus: As above, but a vegetable-draining colander is placed above the stainless-steel pot. The colander is fitted with a 12 inch coffee filter. The solvent and biomass is poured into the colander/pot.

-------------------------------------------------------------------------------What are some good algorithms? Disclaimer: I am only combining things that I have read here and there. These methods are rather crude, so feel free to refine them. I am trying to avoid any methods (apart from the THC extraction) involving the heating of non-polar solvents; I will allow someone with experience in chemistry to elaborate in that area. DMT: First of all, this is what not to do: Boil your biomass, filter, and slowly boil away the water to attempt a one step smokable form. I believe this is not possible. At least with fresh Phalaris arundinacea and dried Desmanthus illinoensis I got a phyto-plastic form that was ridiculously close to the original mass. It is like trading one matrix for another that is excruciating to work with. A more rational approach: if the material is dry one should grind the plant material as finely as possible with a blender or coffee grinder. One can then soak the biomass in a non-polar solvent for a few days, discard the solvent, and dehydrate (dry) the biomass. Then this can be soaked in one of the aforementioned alcohols for a week and filtered. The solvent is saved and more solvent is added to the biomass and after a day, filter and repeat. Finally, do this one more time and after an hour, filter, discard the biomass, and combine the solvents in a pyrex dish and evaporate. You may need to redissolve in hot water, basify to 9 or 10, add a non-polar solvent, and extract the solvent layer weekly for 3 weeks. If the material is not dry grind the plant material, put in a slow cooker with a solution of 2/3 water and 1/3 lemon juice, cook on low for 12 hours, and filter. Evaporate the solution until it is of a quantity that is managable to work with (lid off). Put the solution in a jar and add a non-polar solvent (about 1/4 the amount of the solution). Shake the jar often - open the lid so that the pressure does not build up. Siphon off the non-polar layer in 3 days and discard. The lye must be prepared seperatly - put some lye in a jar, add water, and wait for it to stop bubbling. Basify to 9 or 10 with the lye solution. Add a non-polar solvent (about 1/5 to 1/4 the amount of solution) and let the jar sit for a week. Shake often (remembering to vent the jar) and at the end of a week, siphon off the solvent layer (top) and save it in a jar. Repeat this 3 more times in 3 more weeks. At the end of this time, combine the solvents together and evaporate in a file:///C|/My%20Shared%20Folder/Books%20&%20Essays/...20-%20Extraction%20and%20synthesis%20of%20drugs.txt (7 of 9)3/31/2004 11:26:40 PM


pyrex baking dish.

-------------------------------------------------------------------------------Mescaline Take a fresh cactus cutting and put it through a centrifuge juicer. After this, add lemon or lime juice to the pulp and run it through a second time. Strain through a paper towel (or cheesecloth) and a coffee filter. Put solution in a large jar and add a non-polar solvent. Add enough lemon juice to acidify the solution to pH 5. Add (about 1/4 the amount of solution) a non-polar solvent, agitate the jar, and after 3 days siphon off the top layer. Discard what you siphon off and basify the solution with a pre-prepared lye solution (see DMT) to pH 9 or 10. Add a non-polar solvent (about 1/5 the amount of solution) and extract the non-polar solvent layers 4 times (once a week). Combine extractions and evaporate in a pyrex baking dish. As I mentioned previously, mescaline has an exception to the general rule of alkaloid solubility; that exception is diethyl ether. If you can obtain it, use it to wash the biomass. This is, from what I have heard, truly magical.

-------------------------------------------------------------------------------THC The easiest method that I have knowledge of is to shred your plant material and soak in acetone for a week, a day, and an hour. Then combine and evaporate after filtration. Soak what is left in loose marijuana. The extract may need to be heated if it is too "gummy". A more complicated version is from the book Cannabis Alchemy by D. Gold. The reflux/soxhlet apparatus mentioned in a previous section is used. Reflux for 3 or 4 hours. The book does not specify the amount of time for soxhleting.

-------------------------------------------------------------------------------Psilocin Grind dried carpophores in a coffee grinder or fresh mushrooms in a blender. Apply the DMT algorithm.

-------------------------------------------------------------------------------LSA (Ergine, La-111) Lysergic Acid amides can be extracted from Baby Hawaiian Wood Rose seeds or Morning Glory seeds. To my knowledge, the LSA content in BHWR seeds is of a ratio of 10/1 to Morning Glory seeds. This ratio does not pertain to weight, but means that 10 Morning Glory seeds equals 1 BHWR seed in LA111 content. The seeds are ground and soaked in a non-polar solvent (500 ml) for 20 minutes. The file:///C|/My%20Shared%20Folder/Books%20&%20Essays/...20-%20Extraction%20and%20synthesis%20of%20drugs.txt (8 of 9)3/31/2004 11:26:40 PM


solution is filtered and the solvent is discarded. The seed mush is evaporated fully and then soaked in one of the above mentioned alcohols for 3 days. The solution is filtered and the alcohol is evaporated. What is left is put into gelatin capsules.

-------------------------------------------------------------------------------Harmaline (using Peganum harmala seeds) Grind seeds to a powder. Three grams is considered one dose. Put in slow cooker on low setting with 1/3 vinegar and 2/3 water. After 12 hours, filter and save the solution while repeating with fresh solvent. Afterwards, filter and combine the extractions in the slow cooker. Evaporate on low setting (lid off) and use razor blade to scrape out extract, which is put into gelatin capsules.

-------------------------------------------------------------------------------References: Psychedelic Shamnism; Jim DeKorne ISBN#1-55950-110-3 Cannabis Alchemey; D. Gold ISBN#0-914171-40-2 Pharmacotheon; Jonathan Ott ISBN#0-9614234-3-9 The Organic Chem Lab Survival Manual; James W. Zubrick ISBN#0-471-57504-6 The Entheogen Review; Issue #4 This document from: Sputnik Drug Information Zone Created 11/21/2000 22:39:40 Modified 11/21/2000 22:48:06 Leda version 1.4.3

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Kitchen Chemistry - Extraction and Synthesis

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