Potassium Carbonate → 1-(3,5-Difluorophenyl)piperazine

Participants

Reaction Steps

Bis(2-chloroethyl)amine hydrochloride (2.07 g, 11.60 mmol) was added to a solution of 3,5-difluoroaniline (1.50 g, 11.62 mmol) in n-BuOH (20 mL). After the resulting solution was refluxed for 48 h, anhydrous potassium carbonate (1.61 g, 11.62 mmol) was added. After being refluxed for another 24 h, the reaction mixture was cooled, partitioned between water and CHCl3, and the aqueous layer was extracted with CHCl3. The combined organic layer was washed with water, dried over Na2SO4, and evaporated to dryness. Et2O and 1 N HCl/EtOH were added to the residue, and the precipitate was filtered to give TC-IV-174 (1.17 g, 30%) as a white solid.

Provenance & Evidence