反应详情

A solution of 5-acetylthiophene-2-carboxylic acid (1.80 g, 10.55 mmol) in pyridine (12 mL) and N,N′-dimethylformamide (12 mL) was treated with 1,1′-carbonyldiimidazole (1.88 g, 11.60 mmol) at 45° C. for 4 hours. 2,3-Diaminobenzamide dihydrochloride (2.36 g, 10.55 mmol) was added and the mixture stirred at ambient temperature overnight. The mixture was concentrated and the residue stirred in ethyl acetate and water, filtered, and the yellow solid washed with water and ethyl acetate and dried to give the title compound (2.91 g, 91%). MS(APCI): 304 (M+1)+.

1. concentrationThe mixture was concentrated
2. stirringthe residue stirred in ethyl acetate
3. filtrationwater, filtered
4. washthe yellow solid washed with water and ethyl acetate
5. customdried