反应详情

温度

0 °C

Add slowly 2-fluoro-5-iodobenzoyl chloride (4.0 g, 14.1 mmol) to a 7 N solution of ammonia in methanol (20 mL, 141 mmol) cooled to 0° C. Stir at 0° C. for 45 min then warm to room temperature and stir 5 h. Add an additional amount of the 7 N solution of ammonia in methanol (20 mL) to the reaction mixture and stir for 15 h. Concentrate, dilute with ethyl acetate (300 mL) and wash twice with water (30 mL) and twice with an aqueous saturated solution of sodium chloride (30 mL). Dry (sodium sulfate), filter, and concentrate. Purify by silica gel chromatography, eluting with 60:40 to 40:60 hexanes:ethyl acetate, to give the title compound as a white solid (3.45 g, 92%).

1. temperaturethen warm to room temperature
2. stirringstir 5 h
3. stirringstir for 15 h
4. concentrationConcentrate
5. additiondilute with ethyl acetate (300 mL)
6. washwash twice with water (30 mL) and twice with an aqueous saturated solution of sodium chloride (30 mL)
7. dry with materialDry (sodium sulfate)
8. filtrationfilter
9. concentrationconcentrate
10. customPurify by silica gel chromatography
11. washeluting with 60:40 to 40:60 hexanes