反应详情

温度

60 °C

To a solution of 3-Iodo-1H-indole-5-carboxylic acid (8.0 g, 27.68 mmol) in DMF (80 mL) was added potassium carbonate (4.2 g, 30.44 mmol) and heated at 60° C. for 5 min. Dimethylsulphite (3.5 g, 27.68 mmol) was added and the resulting mixture was stirred at 80° C. for 1 h. The reaction mixture was then added ice cold water and extracted with EtOAc (240 mL). The organic layer was dried over Na2SO4, filtered, concentrated to dryness. The crude solid was washed with n-pentane to obtain the title compound (8.0 g, 95%) as a white solid. MS (ESI, pos. ion) m/z: 299.9 (M−1).

1. extractionadded ice cold water and extracted with EtOAc (240 mL)
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated to dryness
5. washThe crude solid was washed with n-pentane