Under nitrogen protection, 2-hydroxypyridine (2.66 g) and triethylamine (NEt3, 4.05 mL) were dissolved in tetrahydrofuran (THF, 80 mL) and cooled in an ice bath. Thionyl chloride (SOCl2, 1.05 mL) was slowly added dropwise to the above solution, and stirring of the reaction mixture was continued for 1 hr after completion of the dropwise addition. Upon completion of the reaction, the mixture was filtered to remove insoluble matter and the solvent was subsequently evaporated under reduced pressure to afford bis(pyridin-2-yl) sulfite (3.02 g, 91% yield).
