反应详情

To a solution of 2-amino-4-nitrobenzoic acid (14.5 g, 79.6 mmol) in 2.0 M of sulfuric acid aqueous solution (398 mL, 796 mmol) was added a solution of sodium nitrite (8.24 g, 0.119 mol) in water dropwise at 0° C. After the addition, the resulting solution was stirred at same temperature for 1 hour, then a solution of potassium iodide (19.8 g, 0.119 mol) in water was added dropwise at 0° C. The resulting mixture was stirred at rt for 72 hours. The precipitate was filtered and washed by water to give the desired product (19.5 g, 83%). LCMS calculated for C7H51NO4(M+H)+: m/z=294.0.

1. additionAfter the addition
2. stirringThe resulting mixture was stirred at rt for 72 hours
3. filtrationThe precipitate was filtered
4. washwashed by water