反应详情

温度

90 °C

To the solution of 3-[2-(3-isopropylphenylamino)ethylamino]benzoic acid methyl ester (0.83 g, 2.7 mmol) prepared above in dry 1,2-dichloroethane (5.0 mL) was added, under nitrogen, 1,1′-carbonyldiimidazole (0.65 g, 4.0 mmol). The mixture was then heated at 90° C. for 24 h. After cooling to room temperature, the mixture was washed with water, diluted HCl, water and brine, then dried over anhydrous Na2SO4 and concentrated. The crude product was obtained after the removal of the solvent and further purified by column chromatography (silica gel, hexanes:ethyl acetate, 9:1) to give methyl 3-[3-(3-isopropylphenyl)-2-oxo-imidazolidin-1-yl]benzoate as colorless needles (0.78 g, 85.7%). MS (ES+) m/z: 339.

1. additionwas added, under nitrogen
2. temperatureAfter cooling to room temperature
3. washthe mixture was washed with water, diluted HCl, water and brine
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated
6. customThe crude product was obtained
7. customafter the removal of the solvent
8. customfurther purified by column chromatography (silica gel, hexanes:ethyl acetate, 9:1)