Methyl iodide → HCID 68674706, compound

Participants

Reaction Steps

Sodium hydride (21 mg, 0.87 mmol) was added to a solution of 2-{2-[5-(3,4-difluorophenyl)-4H-1,2,4-triazol-3-yl]ethyl}-4-(2,2-dimethylbutyl)-N,N-dimethyl-1H-imidazole-1-sulfonamide (135 mg, 0.29 mmol) in DMF (4 mL) at 0° C., and the reaction was stirred at rt for 30 min. Methyliodide (0.09 mL, 1.4 mmol) was added and stirring continued for 1 hr. The reaction mixture was partitioned between water and diethyl ether. The organic phase was washed with water and brine, dried (sodium sulfate) and concentrated to give a residue. Chromatography of the residue over silica gel (eluting with 60-100% ethyl acetate/hexane) afforded 2-{2-[3-(3,4-difluorophenyl)-1-methyl-1H-1,2,4-triazol-5-yl]ethyl}-4-(2,2-dimethylbutyl)-N,N-dimethyl-1H-imidazole-1-sulfonamide as an off-white solid.

Provenance & Evidence