反应详情

温度

100 °C

2-oxo-2,3-dihydro-1H-benzoimidazole-5-carboxylic acid methyl ester (3.00 g, 15.6 mmol) and phosphorus oxychloride (30 mL) were combined and heated to 100° C. for 48 h. The mixture was cooled to 23° C. and concentrated under reduced pressure. The residue was cooled to 0° C., and cold, saturated aqueous NaHCO3 (60 mL) was added cautiously. After stirring at 23° C. for 15 min, the mixture was sonicated and the resulting residue was filtered to yield the titled compound (3.13 g, 95%), which was used in the next step without further purification. MS (ESI/CI): mass calcd. for C9H7ClN2O2, 210.02; m/z found, 211.0 [M+H]+.

1. temperatureThe mixture was cooled to 23° C.
2. concentrationconcentrated under reduced pressure
3. temperatureThe residue was cooled to 0° C.
4. additioncold, saturated aqueous NaHCO3 (60 mL) was added cautiously
5. customthe mixture was sonicated
6. filtrationthe resulting residue was filtered