反应详情

温度

0 °C

Add at 0° C. a solution of sodium nitrite (2.0 g, 28.9 mmol) in water (15 mL) to a suspension of 3-bromo-4-fluorophenylamine (5.0 g, 26.3 mmol) in a 6 N aqueous solution of hydrochloric acid (25 mL) at 0° C. slowly over 10 min. Stir the mixture at 0° C. for 5 min. Add this solution to a solution of potassium iodide (4.37 g, 26.3 mmol) in water (125 mL) via syringe at 0° C. under nitrogen over 15 min. Stir at 0° C. for 30 min. Warm to room temperature. Extract with four times with dichloromethane (100 mL), dry (sodium sulfate), filter, and concentrate. Purify by silica gel chromatography, eluting with 100:0 to 95:5 hexanes:ethyl acetate to give the title compound as a colorless oil (5.83 g, 74%).

1. stirringStir at 0° C. for 30 min
2. temperatureWarm to room temperature
3. extractionExtract with four times with dichloromethane (100 mL)
4. dry with materialdry (sodium sulfate)
5. filtrationfilter
6. concentrationconcentrate
7. customPurify by silica gel chromatography
8. washeluting with 100:0 to 95:5 hexanes