反应详情

To a mixture of 4-bromo-3-chloro-2-methyl aniline hydrochloride (1.0 g), sodium acetate (0.5 g), and acetic acid (15 mL) was added N-iodosuccinimide (1.0 g) under water-cooling. The reaction mixture was stirred at room temperature for 3.5 hours. To the reaction mixture were added ethyl acetate and water, and alkalified by adding potassium carbonate. Then, a liquid-separation operation was carried out, and the organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10) to obtain 4-bromo-3-chloro-6-iodo-2-methylaniline (1.3 g).

1. temperaturecooling
2. washthe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customevaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10)