Abstractdl‐Nornicotine‐2′‐14C was synthesized in four steps. Nicotinic acid (carboxyl‐14C) was first esterified with diazomethane to yield methyl nicotinate (carboxyl‐14C). The ester was condensed with 3‐lithio‐N‐trimethylsilyl‐2‐pyrrolidone to give 3‐nicotinoyl‐N‐trimethyslsilyl‐2‐pyrrolidone (ketone carbonyl‐14C), which was hydrolyzed and decarboxylated in concentrated hydrochloric acid to give myosmine‐2′‐14C.Reduction of myosmine‐2′14C gave nornicotine‐2′‐14C. Reaction of nornicotine‐2′‐14C in hydrochloric acid with sodium nitrite gaveN′‐nitrosonornicotine‐2′‐14C. Purification of labelled myosmine, nornicotine, andN′‐nitroso