反应详情

5-Chloro-2-(2-nitrovinylamino)benzoic acid (Compound of step 1, 24 g, 98.36 mmol) and potassium acetate (19.2 g, 196.72 mmol) in acetic anhydride (120 mL, 1200 mmol) were stirred for 3 hours at 120° C. The precipitate was filtered, washed with acetic acid and water and dried in vacuo to obtain the title compound. Yield: 15 g (64%); 1H NMR (DMSO-d6, 300 MHz): δ 13.142 (s, 1H), 9.32 (s, 1H), 8.159-8.166 (d, 1H, J=2.1 Hz), 7.822-7.859 (dd, 1H, J=8.7 Hz, 2.4 Hz), 7.734-7.763 (d, 1H, J=8.7 Hz); MS: m/z 225 (M+).

1. filtrationThe precipitate was filtered
2. washwashed with acetic acid and water
3. customdried in vacuo