Abstract: In this paper, a new method for the efficient solid-phase synthesis of nicotine compounds has been developed. A polystyrene-supported sulfonyl chloride resin was prepared from cross-linked polystyrene-supported sulfonic acid resin as a solid-phase organosulfur reagent. Starting from 3-bromopyridine, five nicotine compounds were synthesized by four-step reactions including lithiation/acylation of pyridine, reduction of carbonyl group, sulfonylation of hydroxyl group, and amination/cyclization of sulfonate with overall isolated yields of 52%−66%, and the structures of the synthesized nicotine compounds were identified by ¹H NMR. The method features high yields, simple operation, recycling and reuse of the resin, and the prospect of application in industrial automation production.