1-Methylpiperazine → HCID 57905936, compound

Participants

Reaction Steps

A solution of 3-bromo-5-iodo-benzoic acid (5.0 g, 15.3 mmol) in 100 mL of thionyl chloride was heated under reflux for 2 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The resulting solid was then dissolved in 100 mL of CH2Cl2. N-Methyl-piperazine (2.5 mL, 22.9 mmol) and DIPEA (5.3 mL, 30.6 mmol) were added and the reaction mixture was stirred at room temperature for 3 h. The resulting solution was concentrated under reduced pressure and the crude material was purified by column chromatography (Isco™ 330 g) using 20% MeOH/EtOAc as eluting solvent to afford 5 g (80%) of (3-bromo-5-iodo-phenyl)-(4-methyl-piperazin-1-yl)-methanone as a white solid.

Provenance & Evidence