反应详情

To a stirred solution of 3-iodo-4,5-dimethoxybenzaldehyde (25.0 g, 85.6 mmol) in CH3CN (800 mL) at room temperature, was added a solution of sulfamic acid (10.65 g, 109 mmol) in H2O (135 mL). To this was added, dropwise, a solution of NaClO2 (12.65 g, 112 mmol) in H2O (135 mL) over 20 min period. After stirring for a further 30 min at room temperature, the solvent was removed in vacuo. The reaction was diluted with 1.0 M aqueous HCl (700 mL) and extracted with EtOAc (3×300 mL). The combined organic layers were washed with brine (600 mL), dried over Na2SO4 and concentrated in vacuo to give 3,4-dimethoxy-5-iodobenzoic acid (26 g). The product was used without further purification.

1. additionTo this was added
2. customthe solvent was removed in vacuo
3. additionThe reaction was diluted with 1.0 M aqueous HCl (700 mL)
4. extractionextracted with EtOAc (3×300 mL)
5. washThe combined organic layers were washed with brine (600 mL)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo