反应详情

To a stirred solution of 2-methyl-4-nitroaniline (500 mg, 3.286 mmol) in acetonitrile and water were added p-toluenesulfonic acid monohydrate (1.875 g, 9.858 mmol), sodium nitrite (453 mg, 6.572 mmol) and potassium iodide (1.363 g, 8.215 mmol). The reaction mixture was stirred for 4 h at room temperature. The mixture dissolved in ethyl acetate and washed with water and brine. The organic layer was dried over magnesium sulfate and filtered. The filtrate removed in vacuo. The crude was purified by column chromatography to give 1-iodo-2-methyl-4-nitrobenzene (812 mg, 94%).

1. washwashed with water and brine
2. dry with materialThe organic layer was dried over magnesium sulfate
3. filtrationfiltered
4. customThe filtrate removed in vacuo
5. customThe crude was purified by column chromatography