反应详情

温度

70 °C

To 77 mmol 2-hydroxy-5-methylsulfamoyl-benzoic acid in 300 ml THF was added 85 mmol CDI and the mixture heated at 70° C. for 1 h. 770 mmol methanol was then added and the mixture was heated at 70° C. for 16 h. The mixture was then cooled to room temperature and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane/dichloromethane 45:45:10) to afford the title compound. MS (m/e): 244.1 ([M−H]−, 100%)

1. temperaturethe mixture was heated at 70° C. for 16 h
2. temperatureThe mixture was then cooled to room temperature
3. concentrationconcentrated in vacuo
4. customThe residue was chromatographed on silica gel (eluant: ethyl acetate/heptane/dichloromethane 45:45:10)