反应详情

温度

50 °C

Meldrum's acid (5.29 g, 36.7 mmol) was added to methyl orthoformate (31 ml), and the mixture was stirred for 2 hours while heating under reflux. The resulting mixture was cooled to 50° C., and 5-fluoro-2-propoxyaniline (4.28 g, 25.3 mmol) and methyl orthoformate (3 ml) were added thereto. The resulting mixture was stirred for 6 hours while heating under reflux. The resulting reaction mixture was then cooled to room temperature, and concentrated under reduced pressure. The residue was recrystallized from methanol to thereby obtain 7.61 g of powdery pale brown 5-[(5-fluoro-2-propoxyphenylamino)methylene]-2,2-dimethyl-[1,3]dioxane-4,6-dione (yield: 93%).

1. temperaturewhile heating
2. temperatureunder reflux
3. stirringThe resulting mixture was stirred for 6 hours
4. temperaturewhile heating
5. temperatureunder reflux
6. customThe resulting reaction mixture
7. temperaturewas then cooled to room temperature
8. concentrationconcentrated under reduced pressure
9. customThe residue was recrystallized from methanol