Methanesulfonyl chloride → HCID 23133422, compound

Participants

Reaction Steps

To a solution of 1-[5-(trifluoromethyl)pyridin-2-yl]piperazine (23 g, 0.099 mol) and TEA (42 mL 0.298 mol) in dry dichloromethane (400 mL) maintained at 0° C. under nitrogen atmosphere, was added methanesulfonylchloride (12.6 g, 0.109 mol) over a period of 20 min. The reaction mixture was stirred at room temperature for 6 h and diluted with water. The organic layer was separated, washed with brine, dried over magnesium sulfate, filtrated and concentrated. The crude product was recrystallized from petrol ether:EtOAc (9:1) to afford the title compound as a solid (27 g, 87% yield). TLC: Rf=0.75 (Chloroform:MeOH; 9:1). 1H NMR (CDCl3, 300 MHz) δ: 2.82 (3H, s), 3.32 (4H, m), 3.79 (4H, m), 6.68) (1H, d, J=9 Hz), 7.68 (1H, d, J=9 Hz), 8.42 (1H, s).

Provenance & Evidence