反应详情

温度

135 °C

4-[2-(4-Bromo-phenyl)-2-oxo-ethylcarbamoyl]-3-(2-methoxycarbonylamino-3-methyl-butyryl)-imidazolidine-1-carboxylic acid tert-butyl ester (723 mg) was dissolved in m-xylenes (6.0 mL) and heated at 135° C. Solid ammonium acetate (500 mg, 6.48 mmol) was added and the reaction was stirred at 135° C. After 45 minutes, the reaction was cooled to room temperature and the volatiles were removed in vacuo. The crude material was purified via silica gel chromatography (eluent: EtOAc w 10% MeOH/hexanes) to yield the product 4-(4-Bromo-phenyl)-3′-(2-methoxycarbonylamino-3-methyl-butyryl)-2′,3′,4′,5′-tetrahydro-1H-[2,4]biimidazolyl-1′-carboxylic acid tert-butyl ester (436 mg): LCMS-ESI+: calc'd for C24H32BrN5O5: 550.4 (M+). Found: 551.2/553.2 (M+H+).

1. temperaturethe reaction was cooled to room temperature
2. customthe volatiles were removed in vacuo
3. customThe crude material was purified via silica gel chromatography (eluent: EtOAc w 10% MeOH/hexanes)