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When neoline is irradiated with ultra-violet light in acetic anhydride solution, the N-alkyl group is replaced by N-acetyl. The scope and limitation of this new photochemical reaction will be discussed in connection with various representatives of aconitum and delphinium alkaloids. The work reported has been done in collaboration with Professor Wiesner and his co-workers at the University of New Brunswick, Fredericton, N.B.