反应详情

温度

100 °C

To a 0° C. mixture of 2-amino-4-fluorobenzoic acid (1.18 g, 7.6 mmol) in 12N hydrochloric acid (2.3 mL) and water (13.7 mL) was added dropwise a solution of sodium nitrite (543 mg, 7.9 mmol) in water (1.2 mL). This resulting diazonium salt solution was stirred 10 min at 0° C. A solution of potassium iodide (1.9 g) in sulfuric acid (450 35 μL) and water (3.2 mL) was added dropwise to the 0° C. solution. The reaction mixture was heated to 100° C. for 2 h then cooled to room temperature. 10% sodium bisulfite solution was added and stirred. The precipitate was filtered, washed with water, air dried and recrystallized from toluene.

1. temperaturethen cooled to room temperature
2. filtrationThe precipitate was filtered
3. washwashed with water, air
4. customdried
5. customrecrystallized from toluene