反应详情

温度

180 °C

A mixture of 2-fluoro-nitrobenzene (33.7 g), 4-chloroaniline (61.0 g) and anhydrous potassium fluoride (13.9 g) was stirred at 180° C. for 10 h. After being cooled to rt, 3 M HCl was added and the mixture was stirred at 100° C. for 30 min. Then cooled to rt, filtered by suction, washed with water to give a brown solid. The solid was dissolved in CH2Cl2 and filtered through a thin pad of silica gel, washed with CH2Cl2. The filtrate was concentrated to dryness, and the residue was recrystallized with 95% ethanol to give 57.0 g of orange solid.

1. temperatureAfter being cooled to rt
2. stirringthe mixture was stirred at 100° C. for 30 min
3. temperatureThen cooled to rt
4. filtrationfiltered by suction
5. washwashed with water
6. customto give a brown solid
7. filtrationfiltered through a thin pad of silica gel
8. washwashed with CH2Cl2
9. concentrationThe filtrate was concentrated to dryness
10. customthe residue was recrystallized with 95% ethanol