HCID 136338459, compound → HCID 135999739, compound

Participants

Reaction Conditions

Reaction Steps

Iron powder (231 mg) was added to [2-bromo-5-({(2-fluoro-4,5-dimethoxyphenyl)-[1-(2-nitrophenyl)-5-oxo-4,5-dihydro-1H-[1,2,4]triazol-3-yl]methyl}amino)benzyl]carbamic acid t-butyl ester (232 mg) and a methanol:acetic acid:water (1:1:1) mixed solvent (24 mL), and the mixture was heated for 18 hours at 60° C. under a nitrogen atmosphere. The solvent in the mixture was distilled off under reduced pressure, and ethyl acetate (100 mL) and water (25 mL) were added to the residue. Sodium hydrogen carbonate was gradually added to the mixture to adjust the pH to 8. After sufficiently shaking the mixture, the organic layer was separated off and dried over anhydrous magnesium sulfate. The mixture was filtered to obtain a filtrate, and the solvent in the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-heptane mixture) to obtain the target compound (147 mg) as an off-white solid.

Provenance & Evidence