反应详情

温度

40 °C

Trans-3-(3-pyridyl)acrylic acid (22.35 g) and N,N′-carbonyldiimidazole (24.54 g) were dissolved in dimethylformamide (300 ml) and stirred at 40° C. for 40 minutes. Then, potassium carbonate (41.4 g) and 2-hydroxyphenethylamine hydrobromide (32.70 g) were added under room temperature and stirred for 1 hour. Insoluble materials were filtered out and the filtrate was concentrated under reduced pressure. Dilute hydrochloric acid was added to the residue under ice-cooling and stirring. The precipitated crystal was filtered out, washed with water, purified by silica gel column chromatography (chloroform:methanol=20:1) and then recrystallized in methanol to yield the titled compound (24.98 g, 62%).

1. stirringstirred for 1 hour
2. filtrationInsoluble materials were filtered out
3. concentrationthe filtrate was concentrated under reduced pressure
4. additionDilute hydrochloric acid was added to the residue under ice-
5. temperaturecooling
6. stirringstirring
7. filtrationThe precipitated crystal was filtered out
8. washwashed with water
9. custompurified by silica gel column chromatography (chloroform:methanol=20:1)
10. customrecrystallized in methanol