1H-1,2,4-Triazole → HCID 22859137, compound

Participants

Reaction Steps

1H-1,2,4-Triazole (0.3 mg) was added portionwise to a stirred dispersion of 60% sodium hydride in oil (0.16 g) in dimethylformamide (15 ml) under ice-cooling in a stream of nitrogen, followed by further stirring for 15 minutes. When the evolution of hydrogen (ceased), (2R,3R)-1,3-bis (1H-1,2,4-triazol-1-yl)-2-(2,4-difluorophenyl)-2-butanol (0.64 g) was added to the mixture. The mixture was stirred for 3 hours at 150° C. After cooling, the reaction mixture was added into ice-water and extracted with ethyl acetate. The extract was washed with water and saturated saline and dried. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (silica gel 30 g, eluent: ethyl acetate/acetone/methanol=5:4:1) to give the title compound (Compound 11, 92 mg) as colorless needles.

Provenance & Evidence