反应详情

Acetic anhydride (185 mL, 1.96 mol) and formic acid (85 mL, 2.22 mmol) were mixed and stirred. Methyl-3-aminothiophene-2-carboxylate (50 g, 0.16 mol) was added to the reaction mixture, followed by stirring for about 3 hours at room temperature. The reaction solvent was removed under reduced pressure. Separately, ammonium formate (90 g, 1.43 mol) and formamide (150 mL, 3.76 mol) were mixed and stirred for about 30 minutes. The synthesized material in the above was added to the resulting reaction solution, followed by stirring 8 hours at 150° C. The reaction solution was cooled to room temperature and stirred for about 12 hours. The generated solid was filtered, and washed with water to obtain the title compound (39 g, 81%).

1. stirringby stirring for about 3 hours at room temperature
2. customThe reaction solvent was removed under reduced pressure
3. stirringstirred for about 30 minutes
4. additionThe synthesized material in the above was added to the resulting reaction solution
5. stirringby stirring 8 hours at 150° C
6. stirringstirred for about 12 hours
7. filtrationThe generated solid was filtered
8. washwashed with water