Things To Remember When Working With Ergot Alkaloids, Lysergic Acid, And LSD These compounds are very sensitive and even unstable. This means that the following steps must be taken to keep from ruining your compound or yield. 1.Always use red or yellow photographic dark room light bulbs during any step of LSD manufacture. Direct sunlight, electric filament, or fluorescent light bulbs (etc.) will hurt the above compounds. Dark room bulbs are cheap and are a must. 2.Keep all forms of H2O out of the reaction. Thoroughly dry all the glass ware to be used. Use a drying tube filled with anhydrous MgSO4 (calcium chloride reacts with amines in an unfavorable way and should not be used). I cant be there to hold your hand and guide you through every step, so unless the formula says to add water, the drying tube should be in use, and after the water addition is over, the drying tube goes back on. This way the reaction is always protected even if it does not need to be. Better safe than sorry. Also, if youre not sure if you should use dry reagents, use dry reagents anyway. Also dry the lysergic acid (as described above) and any other precursors in whatever drying process required for that compound before use. Dry the finished LSD or even any intermediate along the way after you have completed the product. Likewise, dry an intermediate that you may have purchased from a chemical supplier. 3.Keep oxidizing agents from these items. Even the oxygen in the air can oxidize some of these compounds. The formula states that during some of the reactions above, an inert gas (nitrogen) must be used for an atmosphere inside the reaction vessel. Nitrogen can be obtained in small bottles (tanks) at a very reasonable fee, without any questions asked. Make sure you use a regulator and introduce a slow stream into the vessel by way of a gas inlet tube or an equivalent. Always flush the vessel before putting any reagents into it (flush the air out with nitrogen). I would use a nitrogen atmosphere from the very beginning of the formula to the very end, even if the formula did not specify its use. Very few of the above formulas call for a nitrogen atmosphere during evaporation, but I feel this may be bad for yield and or potency. LSD has many doses per gram, and if you lose 1/2 g because you were too cheap to use three dollars worth of nitrogen, you have lost about 2,000 doses at $5 a dose = $10,000 of LSD wasted. Better safe than sorry? Also, any precursors you make or buy should be stored in a nitrogen atmosphere, as should LSD. This can be done by poking a gas inlet tube into the vessel trust above or a little below the substance) flushing the air out with a moderate stream of nitrogen then quickly reinstall the cap or stopper. The best way to store LSD is by producing it in the maleate form. This not only makes it resistant to oxidation, but it purifies it, too. Use the procedure above (JOC, 24, 368, or CA, 57, 5979) when you get to the last dry-and-evaporate-in-vacuo step, then treat the residue as specified. 4.Never subject these compounds to excessive heat, or any type of temperature warmer than the inside of your refrigerator. Even LSD maleate will decompose in excess heat, so store in a refrigerator. Keep evaporation procedures cooled. This will slow the evaporation process down, but that is better than losing the product. Some of the above formulas require heat for a reaction. This is Ok, but do not exceed the temp stated at any time and never heat longer than needed. Also, nitrogen atmospheres are used during heating operation. Substituents LSD analogs (lysergic acid amides) can be prepared by substituting amines in place of diethylamine. The potency usually drops anywhere from 33% to 75% depending on the substituent. Diethylamine is highly suspicious, and the substituent will produce a lysergamide that is most likely legal, as legislation has only singled out lysergic acid diethylamide. Little work has been done on the potency of substituted Iysergamides, so a little experimentation by you may be in order. Personally, I would like to try substituting a potent phenethylamine or phenylisopropylamine such as DOM (STP) or 4-bromo-2,5-dimethoxyamphetamine. If I could get a government grant, or maybe a grant from a major pharmaceutical corporation, like Upjohn or Lilly, then I could play around with such experiments. The following substituents give lysergamides with potencies as indicated in doses per gram (remember that LSD gives about 6,000 to 9,000 doses): Ethylpropylamine 2,000 to 5,000 Morpholide 600 to 2,000 Methylpropylamine 600 to 1,000 Dipropylamine 600 to 1,000 Methylethylamine 400 to 600 Dimethylamine 300 to 400 Pyrrolidide 300 to 400 As a point of reference, DOM (STP) is one of the most powerful amphetamines, at 200 doses per gram. At $5 a line, its value is about 5 times 200 = $1,000 a gram. For more info see JMC, 16, 532 (1973). Claviceps purpurea is not the only place to get d-lysergic amides. The plant group of Convolvulacea has been found to posses lysergic acid amides such as ergine and several others. These Convolvulacea type of plants do not cause the dreaded St. Anthonys fire, as does claviceps purpurea, and as a matter of fact, they are hallucinogenic if eaten in large doses. Care must be taken that the seeds have not been treated with poison to discourage usage as a mind alterant, or treated with methyl mercury to prevent spoilage. When these seeds are to be used for LSD syntheses, make sure to clean off the white layer that surrounds them by singeing or mild burning. Also, ask for Hawaiian Rose Wood, as these are the only ones that contain an appreciable amount of lysergic related compounds. These compounds must be extracted as below, hydrolyzed (like ergotamine) as above, and then used in any of the formulas that require d-lysergic acid or possibly used directly in the Hofmann hydrazine method; CA, 57, 12568 (1962). These seeds have very little amide, so you can plan on quite a lot of work in the extraction step. According to A. Hoffer and H. Osmond, the most amide plentiful species (Woodrose) has a minute 3 to 6 mg of amide per every gram of seed. This means that if you extract very thoroughly, you will require a little over 200 g of seeds to get 1 g of amide, which will be reduced further after hydrolysis to give you about 0.5 g of usable d-lysergic acid. Extract as follows. Pulverize the seeds in a clean blender until they are a fine powder. Put this powder into a beaker, add 1 1iter of petroleum ether to every 900 to 1000g of powdered seeds, stopper the beaker to prevent evaporation and let set for 3 days. Filter off the petroleum ether and let evaporate to make sure no amides were extracted (there should not be much, if any) from the ether. Add 1 1iter of methanol (dry is best) and let soak for 4 days with vigorous shaking, now and then. Filter off the methanol and evaporate it under vacuo (vacuum speeds the process). In the meantime, add 500 ml of fresh methanol to the powder and extract it again for 3 or 4 days. Filter as before and extract again with about 300 ml of methanol. Combine the residues of all extractions and hydrolyze.
Posted on: Tue, 25 Mar 2014 00:35:52 +0000
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