反应详情

5-Methyl-2-(2-nitrovinylamino)benzoic acid (Compound of step 1, 1.5 g, 6.756 mmol) and potassium acetate (1.3 g, 13.51 mmol) were stirred in acetic anhydride (8 ml, 148 7 mmol) for 3 hours at 120° C. The precipitate was filtered and washed with acetic acid until the filtrate is colorless and then washed with water and dried in vacuo to obtain the title compound. Yield: 610 mg (64%); 1H NMR (DMSO-d6, 300 MHz): δ 9.126 (s, 1H), 8.035 (s, 1H), 7.606 (s, 2H), 2.432 (s, 3H); MS: m/z 203 (M−1).

1. filtrationThe precipitate was filtered
2. washwashed with acetic acid until the filtrate
3. washwashed with water
4. customdried in vacuo