反应详情

温度

-10 °C

To a solution of 2-thiazolecarboxaldehyde (500 mg, 3.87 mmol) in 35 mL of pyridine, 1-(2-amino-4-methoxyphenyl)ethanone (640 mg, 3.87 mmol) was added and the solution was cooled to −30° C. before POCl3 (750 μl, 8.13 mmol) was added drop wise. The reaction mixture was stirred at −10° C. for 1 hour and then at room temperature for 2 hours. The mixture was concentrated under vacuum and the residue was triturated with NaHCO3 to pH 7. The precipitate was filtrated, washed with water and dried. The amide was pure enough for the next step without purification (972 mg, 91%).

1. additionwas added drop wise
2. waitat room temperature for 2 hours
3. concentrationThe mixture was concentrated under vacuum
4. customthe residue was triturated with NaHCO3 to pH 7
5. filtrationThe precipitate was filtrated
6. washwashed with water
7. customdried
8. customThe amide was pure enough for the next step without purification (972 mg, 91%)