Water → HCID 18960027, compound

2,5-Difluoroaniline (38 g) was dissolved in acetic acid (120 ml), and then pyridine (25 g) was added thereto, followed by stirring. A mixed solution of iodine monochloride (50 g) with acetic acid (30 ml) was added dropwise thereto. After stirring at room temperature for 1 hour, the mixed 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 distilled off chloroform therefrom. The residue was distilled under reduced pressure (b.p. 130° to 140° C./20 mmHg), and then recrystallized from methanol, to give 4-iodo-2,5-difluoroaniline (50 g).

1. stirringAfter stirring at room temperature for 1 hour
2. stirringthe mixed solution was further stirred at 70° to 80° C. for 2 hours
3. filtrationthe precipitated crystals were filtered
4. washby washing with water
5. dissolutionThe resulting crystals were dissolved in chloroform
6. washwashed with water twice
7. distillationby distilled off chloroform
8. distillationThe residue was distilled under reduced pressure (b.p. 130° to 140° C./20 mmHg)
9. customrecrystallized from methanol

ORD record

ord-862af2edb0474ad0b950fa0f9ce78f1e

Source dataset

uspto-grants-1994_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05356558