反应详情

温度

60 °C

Iron powder (70 mg) was added to [2-bromo-5-({[3-(2-dimethylaminoethoxy)-5-ethyl-2-fluorophenyl]-[1-(2-nitrophenyl)-5-oxo-4,5-dihydro-1H-[1,2,4]triazol-3-yl]methyl}amino)benzyl] carbamic acid t-butyl ester trifluoroacetic acid salt (76 mg) and a methanol:acetic acid:water (1:1:1) mixed solvent (6 mL) under a nitrogen atmosphere, and the mixture was heated for 18 hours at 60° C. 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 reverse-phase high performance liquid chromatography (acetonitrile/water mixed solvent, 0.1% trifluoroacetic acid) to obtain the target compound (44 mg) as a colorless oil.

1. filtrationThe mixture was filtered
2. customto obtain a filtrate
3. distillationthe solvent in the filtrate was distilled off under reduced pressure
4. customThe residue was purified by reverse-phase high performance liquid chromatography (acetonitrile/water mixed solvent, 0.1% trifluoroacetic acid)