Baeocystin (7) (4‐phosphoryloxy‐N‐methyltryptamine) has been synthesized starting from 2‐methyl‐3‐nitrophenol (1). The spectral data (UV, IR, 1H‐, 31P‐, 13C‐NMR, MS) are identical with those of 7 isolated from Psilocybe semilanceata.

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The content of tryptamine derivatives in Psilocybe semilanceata, a popular hallucinogenic mushroom, was measured by high-performance liquid chromatography. Most of the 52 samples have been collected at several localities in Switzerland during a 1-5 year period. The content of psilocybin and baeocystin varied in the range of 0.21-2.02% and 0.05-0.77%, respectively, whereas only traces of psilocin were present. The variability of the alkaloid level depending on origin, year of collection, size and part of mushrooms is discussed.