反应详情

5-Fluorosalicylaldoxime (20.2 g, 0.13 mol) was dissolved in acetic anhydride (100 ml), followed by refluxing for 5 hours, distilling off acetic anhydride under reduced pressure after completion of the reaction, adding to the remaining oily material, a solution of KOH (20 g) dissolved in water (100 ml) and ethanol (100 ml), heating the mixture at 80° C. for 2 hours, allowing to cool down to room temperature, adding 6N-hydrochloric acid (50 ml) and water (200 ml) to deposit crystals, filtering the crystals, and recrystallizing from methanol (30 ml) to obtain acicular crystals (15.6 g). M.p. 121°~122° C.

1. temperatureby refluxing for 5 hours
2. distillationdistilling off acetic anhydride under reduced pressure
3. customafter completion of the reaction
4. additionadding to the remaining oily material
5. filtrationfiltering the crystals
6. customrecrystallizing from methanol (30 ml)