This is taken from CA, 57, 5979 (1962). It is designed by Hofmann to give 1-methyl-D-lysergic acid, and is modified to give LSD and iso-LSD. Dissolve 0.54 g of lysergic acid in 10 ml of freshly distilled phosphorous oxychloride, stir 0.42 g of powdered, fresh phosphorous pentachloride. Allow to stand at room temp for 2 min, then at 90° for 2 min, then evaporate in vacuo. Extract the residue with hexane to give lysergic acid chloride hydrochloride. To save time you may extract the reaction mixture without evaporating. Add 2.5 g of the hydrochloride to a cooled solution of 7 ml of diethylamine (or analog) in 25 ml of methylene chloride that is cooled to 0°. Note: This solution is cooled to 0° before the addition. With stirring add 13.75 ml of dry pyridine and stir for 30 min with cooling to keep the temp at 0° or a little below. Warm to room temp and continue the stirring for 90 min. Evaporate in vacuo to get the LSDs. Separate as already described.
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