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ing in the cold before then adding 25 ml of diethylamine. Stir for an additional 10 minutes, then pour the batch into a 2000 ml sep funnel. Now to the sep funnel add 800 ml of water. Mix this in thoroughly, then add 400 ml of saturated salt solution in water. Mix this in, then extract out the LSD by repeated extraction with 250 ml portions of ethylene dichloride. Check with a blacklight for complete extraction.
6 LSD From Lysergic Acid And SO3 55 The combined ethylene dichloride extracts should be evaporated under a vacuum as above, and the residue of LSD and iso-LSD should be separated and treated as above. 7 LSD From Lysergic Acid And Trifluoroacetic Anhydride 51 1 LSD From Lysergic Acid And Trifluoroacetic Anhydride This method is a little bit lame, but it may be the method of choice if trifluoroacetic anhydride or trifluoroacetic acid should happen to fall from the sky into one's hands. The reason why this method is a bit lame is threefold. Anhydrous lysergic acid is required for this reaction.
To obtain anhydrous lysergic acid, the lysergic acid hydrate yielded by the methods in Chapter 5 must be baked under high vacuum for a couple hours. This is obviously not good for such a delicate molecule. The water molecule will be shed by a baking temperature of 120° C at a vacuum of 1 mm Hg, 140° C at 2 mm Hg, and still higher temperatures at less perfect vacuums. A MacLeod gauge is the only instrument that I know of which is capable of accurately measuring such high vacuums. Another reason why this method is lacking is that the yields are not so good as those achieved by the other synthetic routes presented in this book. It is possible to recover the unreacted lysergic acid at the end of the process, but this does not make up for the initial lower yield, not to mention the added hassle of recovering and redrying the lysergic acid. Strike number three for this route is its propensity to give byproducts that are difficult to separate from the desired product. I am Practical LSD Manufacture 58 not talking here about the large amount of iso-LSD that this method makes. That molecular jumbling is inconsequential, because the lysergic acid used is itself an isomeric mixture. Rather, what can occur here is the production of LSD and other by-products.
The mechanics of this reaction are similar to the reaction with SOs, in that two molecules of the anhydride react with the lysergic acid molecule to form the mixed anhydride. In this reaction, there is no need to first react the lysergic acid with hydroxide to form the metal salt. Also, the need to follow exact stoichiometric quantities of reactants is not as pressing as in the SO$ method. To do the reaction, into a 1000 ml flask (carefully dried and equipped with a magnetic stirring bar) place 16 grams of lysergic acid and 375 ml of acetonitrile. The lysergic acid will not dissolve. Stopper the flask and place it in the freezer to cool the contents to -20f

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