Abstract Efficient procedures were developed for N-deethylation of lappaconitine to give N (20)-deethyllappaconitine. Alkyl derivatives of N (20)-deethyllappaconitine, including labeled lappaconitine, and N (20)-acetoxy-N (20)-deethyllappaconitine were prepared for the first time. The assignments of the signals for the carbon atoms in the 13 C NMR spectra of lappaconitine and related lappaconine were refined using 13 C—13 C 2D ...