反应详情

Acetic anhydride (57 mL, 0.6 mol) was added slowly, over approximately 40 min, to stirred 2-fluoroaniline (27, 55.7 g, 0.5 mol) under cooling (water bath) to maintain the reaction temperature at 60° C. to 70° C. After 10 hours more, the reaction mixture was poured into H2O, the whole was extracted with ethyl acetate (2×300 mL). The combined organic extracts were washed with 5% aqueous NaHCO3, brine, dried (K2CO3), filtered and concentrated to provide the title compound as a white solid (67.0 g, 88%).

1. temperatureto maintain the reaction temperature at 60° C. to 70° C
2. extractionthe whole was extracted with ethyl acetate (2×300 mL)
3. washThe combined organic extracts were washed with 5% aqueous NaHCO3, brine
4. dry with materialdried (K2CO3)
5. filtrationfiltered
6. concentrationconcentrated