反应详情

To a solution of 5-(3,6-bis-allyloxybenzo[d]isoxazol-5-yl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (0.055 g, 0.15 mmol) in EtOH (4 mL) is added tetrakis(triphenylphosphine)palladium(0) (0.005 g, 0.004 mmol). The mixture is stirred for 5 min at room temperature, at which point potassium carbonate (0.056 g, 0.405 mmol) is added. The mixture is stirred at room temperature for 5.5 h. The solvent is removed under reduced pressure and the crude product is purified by chromatography on a Biotage purification system eluting with a gradient of water/CH3CN to afford 5-(3-allyloxy-6-hydroxybenzo[d]isoxazol-5-yl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one as a solid: (M−H)−=324.0.

1. additionis added
2. customThe solvent is removed under reduced pressure
3. customthe crude product is purified by chromatography on a Biotage purification system
4. washeluting with a gradient of water/CH3CN