反应详情

To acetic anhydride (74.2 g, 727 mmol) was added formic acid (32.9 mL, 872 mmol) under a nitrogen atmosphere while stirring at room temperature, followed by stirring at 70° C. for 3 hours. The reaction mixture was allowed to cool down to room temperature, and tetrahydrofuran (50 mL) was added. To the solution was added a solution of 2-bromoaniline (50.0 g, 291 mmol) in tetrahydrofuran (50 mL) at room temperature, followed by stirring at the same temperature for 1 hour, and concentration was carried out. To the resultant crude crystals was added ethanol (200 mL), followed by heating and stirring at 60° C. After the crystals dissolved, the mixture was allowed to cool down to room temperature, then water (400 mL) was added, followed by stirring for 3 hours. The precipitated crystals were collected by filtration to give 48.8 g of the title compound as white crystals.

1. stirringby stirring at 70° C. for 3 hours
2. temperatureto cool down to room temperature
3. stirringby stirring at the same temperature for 1 hour
4. concentrationconcentration
5. additionTo the resultant crude crystals was added ethanol (200 mL)
6. temperatureby heating
7. stirringstirring at 60° C
8. dissolutionAfter the crystals dissolved
9. temperatureto cool down to room temperature
10. additionwater (400 mL) was added
11. stirringby stirring for 3 hours
12. filtrationThe precipitated crystals were collected by filtration