反应详情

26.5 g (0.109 mol) of 5-chloro-2-[2-nitro-ethylideneamino]-benzoic acid (Example 23a) in 116 ml acetic anhydride are heated and kept at 110° C. 12.92 g (0.131 mol) potassium acetate are added in 2 min and heating is continued for 40 min at 130-135° C. After 10 min, the title compound starts to crystallize. The reaction vessel is cooled to rt and the solid filtered off and washed with acetic acid and water. Drying follows at 95° C. for 16 h (high vacuum). mp: 341-342° C. (dec.). MS: 225 (M++1); HPLC: tret=7.33 min (Grad 1).

1. customkept at 110° C
2. temperatureheating
3. waitAfter 10 min