反应详情

2,6-Difluoroaniline (38 g) was dissolved in acetic acid (120 ml), and then pyridine (25 g) was added thereto, followed by stirring. Then, a mixture of iodine monochloride (50 g) with acetic acid (30 ml) was added dropwise thereto. After stirring at room temperature for 1 hour, the reaction solution was further stirred at 70° to 80° C. for 2 hours. Then, the reaction solution was poured into water, and the precipitated crystals were filtered, followed by washing with water. The resulting crystals were dissolved in chloroform, and then washed with water twice, further with 10% potassium hydroxide aqueous solution twice, and furthermore with water twice, followed by distilling off chloroform. The residue was distilled under reduced pressure (b.p. 120° to 130° C./20 mmHg), and then recrystallized from methanol to give 4-iodo-2,6-difluoroaniline (44 g).

1. additionwas added dropwise
2. stirringAfter stirring at room temperature for 1 hour
3. stirringthe reaction solution was further stirred at 70° to 80° C. for 2 hours
4. filtrationthe precipitated crystals were filtered
5. washby washing with water
6. dissolutionThe resulting crystals were dissolved in chloroform
7. washwashed with water twice
8. distillationby distilling off chloroform
9. distillationThe residue was distilled under reduced pressure (b.p. 120° to 130° C./20 mmHg)
10. customrecrystallized from methanol