from "Psychedelic Guide to the Preparation of the Eucharist" by Robert Brown, 1967.
--------------------------------------------------------------------------------
Preparatory arrangements:
Starting material may be any lysergic acid derivative, from ergot on rye grain or from culture, or morning glory seeds or from synthetic sources. Preparation #1 uses any amide, or lysergic acid as starting material. Preparations #2 and #3 must start with lysergic acid only, prepared from the amides as follows:
10 g of any lysergic acid amide from various natural sources dissolved in 200 ml of methanolic KOH solution and the methanol removed immediately in vacuo. The residue is treated with 200 ml of an 8% aqueous solution of KOH and the mixture heated on a steam bath for one hour. A stream of nitrogen gas is passed through the flask during heating and the evolved NH3 gas may be titrated is HCl to follow the reaction. The alkaline solution is made neutral to congo red with tartaric acid, filtered, cleaned by extraction with ether, the aqueous solution filtered and evaporated. Digest with MeOH to remove some of the coloured material from the crystals of lysergic acid.
Arrange the lighting in the lab similarly to that of a dark room. Use photographic red and yellow safety lights, as lysergic acid derivatives are decomposed when light is present. Rubber gloves must be worn due to the highly poisonous nature of ergot alkaloids. A hair drier, or, better, a flash evaporator, is necessary to speed up steps where evaporation is necessary.
Preparation #2
Step I. Use Yellow light
5.36 g of d-lysergic acid are suspended in 125 ml of acetonitrile and the suspension cooled to about -20 C in a bath of acetone cooled with dry ice. To the suspension is added a cold (-20 C) solution of 8.82 g of trifluoroacetic anhydride in 75 ml of acetonitrile. The mixture is allowed to stand at -20 C for about 1.5 hours during which the suspended material dissolves, and the d-lysergic acid is converted to the mixed anhydride of lysergic and trifluoroacetic acids. The mixed anhydride can be separated in the form of an oil by evaporating the solvent in vacuo at a temperature below 0 C, but this is not necessary. Everything must be kept anhydrous.
Step II. Use Yellow light
The solution of mixed anhydrides in acetonitrile from Step I is added to 150 ml of a second solution of acetonitrile containing 7.6 g of diethylamine. The mixture is held in the dark at room temperature for about 2 hours. The acetonitrile is evaporated in vacuo, leaving a residue of LSD-25 plus other impurities. The residue is dissolved in 150 ml of chloroform and 20 ml of ice water. The chloroform layer is removed and the aqueous layer is extracted with several portions of chloroform. The chloroform portions are combined and in turn washed with four 50 ml portions of ice-cold water. The chloroform solution is then dried over anhydrous Na2SO4 and evaporated in vacuo.